Water → HCID 54222524, 화합물

HRID 1736619노트

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HRID 1736619 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH:16]=[CH:17][CH:18]=[CH:19][C:20]([O:22]C)=[O:21])=[O:7])([CH3:4])([CH3:3])[CH3:2].[Na].O>CO>[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH:16]=[CH:17][CH:18]=[CH:19][C:20]([OH:22])=[O:21])=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 962WaterHCID 5360545SodiumHCID 54280683HCID 54280683, 화합물

생성물 1

HCID 54222524HCID 54222524, 화합물수율 86%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

A stirred mixture of 0.85 g (2.7 mmol) of methyl 5-[2-(tertbutoxycarbonylaminomethyl)phenyl]-2,4-pentadienoate, 1.17 g (11 mmol) of sodium carbinate, 15 ml of water and 15 ml of methanol was heated at reflux for 2 hours. After the produced methanol was distilled off, the solution was cooled to 0° C. and carefully acidified with 1N hydrochloric acid. The resulting mixture was extracted with methylene chloride and the extracts were washed with brine, dried (Na2SO4) and concentrated. Recrystallization of the residue from 1:3 methylene chloride:hexane gave 0.7 g (86%) of the product as crystals, mp 179°-182° C. (dec).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 hours
  3. distillationAfter the produced methanol was distilled off
  4. extractionThe resulting mixture was extracted with methylene chloride
  5. washthe extracts were washed with brine
  6. dry with materialdried (Na2SO4)
  7. concentrationconcentrated
  8. customRecrystallization of the residue from 1:3 methylene chloride

출처 및 근거

ORD 기록
ord-ae6ca78356274f5f9d1e33654293a8d4
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05541286

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