HCID 86742261、化合物 → HCID 20132436、化合物

HRID 845220ノート

反応式

HRID 845220 の反応式
[Cl:1][C:2]1[CH:27]=[CH:26][C:5]([CH:6]([C:14]2[CH:15]=[C:16]([CH:23]=[CH:24][CH:25]=2)/[CH:17]=[CH:18]/[C:19]([O:21]C)=[O:20])[N:7]2[CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)=[CH:4][CH:3]=1>CO.[OH-].[K+]>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:6]([C:14]2[CH:15]=[C:16]([CH:23]=[CH:24][CH:25]=2)/[CH:17]=[CH:18]/[C:19]([OH:21])=[O:20])[N:7]2[CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)=[CH:26][CH:27]=1

参加物

4

反応物 1

HCID 86742261HCID 86742261、化合物

生成物 1

HCID 20132436HCID 20132436、化合物収率 46%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

The ester from above (1.05 g, 2.73 mmol) was dissolved in 20 mL of methanol with 8 mL of 1M potassium hydroxide and stirred overnight at room temperature. The methanol was removed in vacuo and the remaining aqueous solution was extracted with two 15 mL portions of ether. The aqueous layer was adjusted to a pH of 7 with 1M hydrochloric acid. The solution was chilled and the white powdery precipitate was collected by filtration to give 504 mg (46%) of (E)-3-(4-chloro-α-(4-methyl-1-piperazinyl)benzyl)cinnamic acid, m.p. 131°-141°. Calc. for C21H23ClN2O2.2H2O: C, 61.99; H, 6.69; N, 6.88; Cl, 8.71. Found: C, 61.98; H, 6.72; N, 6.89; Cl, 8.66.

後処理

  1. customThe methanol was removed in vacuo
  2. extractionthe remaining aqueous solution was extracted with two 15 mL portions of ether
  3. temperatureThe solution was chilled
  4. filtrationthe white powdery precipitate was collected by filtration

出典と根拠

ORDレコード
ord-ed3e99f54e074df78f952d9645a28d95
出典データセット
uspto-grants-1988_07
特許番号
US04757074

反応ノート

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