Trifluoroacetic acid → 4-Methyl-4-(p-nitrobenzyloxycarbonyl)aminovaleric acid

HRID 1252222

반응식

HRID 1252222 반응식
COC1C=CC(C[O:8][C:9](=[O:29])[CH2:10][CH2:11][C:12]([CH3:28])([NH:14][C:15]([O:17][CH2:18][C:19]2[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=2)=[O:16])[CH3:13])=CC=1.C1(OC)C=CC=CC=1.FC(F)(F)C(O)=O>C(OCC)C>[CH3:28][C:12]([NH:14][C:15]([O:17][CH2:18][C:19]1[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=1)=[O:16])([CH3:13])[CH2:11][CH2:10][C:9]([OH:29])=[O:8]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 539719334-Methyl-4-p-nitrobenzyloxycarbonylaminovaleric acid p-methoxybenzyl ester

생성물 1

HCID 133343844-Methyl-4-(p-nitrobenzyloxycarbonyl)aminovaleric acid

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A mixture of 4-methyl-4-p-nitrobenzyloxycarbonylaminovaleric acid p-methoxybenzyl ester (25 g), anisole (25 g) and trifluoroacetic acid (125 ml) was stirred for 15 minutes at room temperature. Evaporation of trifluoroacetic acid gave an oily residue which was then dissolved in diethyl ether. The ether solution was extracted with aqueous sodium carbonate. The aqueous layer was washed with diether ether, acidified with dilute hydrochloric acid and extracted with benzene. The benzene extract was washed with water, dried over anhydrous sodium sulfate and evaporated to give 4-methyl-4-p-nitrobenzyloxycarbonylaminovaleric acid.

후처리

  1. customEvaporation of trifluoroacetic acid
  2. customgave an oily residue which
  3. extractionThe ether solution was extracted with aqueous sodium carbonate
  4. washThe aqueous layer was washed with diether ether
  5. extractionextracted with benzene
  6. extractionThe benzene extract
  7. washwas washed with water
  8. dry with materialdried over anhydrous sodium sulfate
  9. customevaporated

출처 및 근거

ORD 기록
ord-ee09b96d6f97420b9c4ef0a3e6050de5
출처 데이터셋
uspto-grants-1988_05
특허 번호
US04742052

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