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1、A 30mL，oenckd， ro-oted fl as quipped wth aanetic rrr， Deatark trp, nd reflux condnse. The fask was harged with 0g (20 mmol) of L-（+）tartarc aci， 6。g （0 ol) of bzy acohl,75 g（0。25 mml) fp-toluenefoni acid monodad 40 mL of tluene Th mxtue was hateue l i an oil bath(out 30）for r.Dungthi erid he theoret
2、il ao ofwat (0。2 mL） was clect.The mixtre ws allowedtol o amenttmpatu, dilt wi ther， adporedinto5 mL ofueus，satuated soiu biaronate. he oanc phase ws seprated andthequeus phsewas etracedwcewih 20 m of eher. Tecombined organic pes er ied ovesodum ulfte。Te solvent was reoedwith arotay evporaor,n he re
3、sulting crude odc ws titurae with hexaneer （20:1， 20mL） to v wite cytals of （）-ibenzyl ttrate. Th ecipitate was colectedby filtration d ahedwth hexneethr (20:) The fltrate warther ccntred to give a secnd co。The otal ield wa。 （9）， 405.5 酰氯和醇、酚的酯化反应示例：酰氯是强酰化剂和醇、酚作用生成酯的反应很迅速，此方法适用于由空间障碍的酯化.经常是在吡啶或其它叔胺参
4、与下反应.I an ovenried，500m, wncked,roun-otodflak eqipp wt amagneticsibarand a rube septum wasplacd 1,3，5-triO-enzl-Drbonose(5。0 g， 10 ）ad 2,6-lutie (。4 g，13.0 mol) in 200 mLf dry dichloromethne der anrgn amspre Te ration mixtue as coole o 0 and3（triluoothyl）bzoyl chloride(3。3 , 6。 mol） as ded dropwi o
5、hestredtion over 30 min fte te addition， herecon mixtre was wamed to romtemperaurand stired ovenigh. Theretnasuenced wi 8mL of aqou satuaed soim bicaront， the pses weesprd and te qeous pase was extacted wthicloromethae （00 mL 2）. ecombined organicextractsee washed wih brine(0 m 2)a dried overandous
6、mgesi sulae。 Afteltrio, th solvnt asremoved nereduced presurgeyelow o Prifiat by flashcolum chomatgrap(140g ofslael)adeutng wih25 thyl aetae in hexas givs awhite solid that can be rcstallizd omEtOAc/hx toyield 1，3,5Orienzoy-2-O( triluormehy）benoyl-D-riuranse （5。2 g， 82) as whi crysls14.Amixtur of 28
7、5g nitrobenzyl hlorie，30.0 g o 3，5-dichlophno ad 300 mL f idine s heatedunder eux fo3 h。Atr ompltio of the rcton， tepyidineas ditild ff under reducedrsse， remaining rection product w isoled ethyl cetate, an he sluon waswashed withwaterand thn with satuatdauous olutionof soi chlorieand concnrted unde
8、educed presue togvcrudecrystal，which was rersalized from ehyl acetatoiv3,5dichlronyl4nitrobnzote （4.2 ) as dle15酯和另一种过量的醇在少量的碱或酸催化下共热，发生烷氧基转移，生成另一种酯。A mixtur of Ethl cyno3，3diphnylacyat （3.1 g，03 mol），lopentanl (1mL） ad Na2CO ( g） wee eated a 15 ith disstilav remova of the ethaol fomed, assisted y a
9、 stram f nitogn Afte abou ， he ractioitue as filtrd hot in rderto rme t Na3.After hefltrte had ben oe, th peciitt hch haformed was ltered of，washedwit etroemeher n ridto give cyloetl cyno3， 3-dpheycrylat (78。1 , 8） s a coloes slid 1.e mxte o 00 g o 3-etyox-7-(-nito-2-pyridil)oy-1Hinde, 5ml of benzoy
10、l hlord and 15 g of poueesuloncacdwas stirrd t . Afer stiring for。5 ，ethyl ceat as aded to the rction ltnd the soution washe iurn ith atua sodm hdogeronatesoution an asatrated siumchlrie solution. he solution tacewth ehylcetat ws dred vr nhydrou manesium sulte ad the solents dstlled off。The rsuting
11、residea puied y silica ge comnhromaorphy （euent: hexne/tylacet=10:1)o obtan 30 mg 3beoylxy-7 （5nit2prdiy） xy1ndene as a whie powdr1. 50m, oeecked ask euipe wh a calim chloide drig b waschagdwth 8。3 g (0.20 mol） o mnoethyl umaate， 00 mof rydcloromethane， 4447 g （0。6 ol) otertbuy lcoh， and .00 g （0.1
12、mol） of dimethylnridine. hesolution was sired acooled ian ce ath to0Cwle 45.59 (.2mol) of dcclhexylbdiimide wa aded 5-inrio。 ter a futher 5 in at 0C he ce bth wa eoved andthedbrown reaction mixte wa sired f 3 ha r teperature。 The icyclohxyur tht has eciitaed wasemoed filtrtio hrough frttdchner fnnl（多孔布氏漏斗) （G3)， antefltate wasashed with two50m rtions o05 N hydrhlorc id 无化 盐酸andto50 mL portos of straed sdium icr
