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

HRID 1252222

反応式

HRID 1252222 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ee09b96d6f97420b9c4ef0a3e6050de5
出典データセット
uspto-grants-1988_05
特許番号
US04742052

関連ノート

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