Water → HCID 54222524、化合物

HRID 1757058ノート

反応式

HRID 1757058 の反応式
[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]

参加物

5

反応物 3

HCID 962WaterHCID 5360545SodiumHCID 54280683HCID 54280683、化合物

生成物 1

HCID 54222524HCID 54222524、化合物収率 86%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

A stirred mixture of 0.85 g (2.7 mmol) of methyl 5-[2-(tert-butoxycarbonylaminomethyl)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).

後処理

  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

出典と根拠

ORDレコード
ord-7b738f3a0dd84c748ba538b0d289c65e
出典データセット
uspto-grants-1995_08
特許番号
US05444048

反応ノート

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