HCID 86742261, 화합물 → HCID 20132436, 화합물

HRID 845220노트

반응식

HRID 845220 반응식
[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

참가 물질

4

반응물 1

HCID 86742261HCID 86742261, 화합물

생성물 1

HCID 20132436HCID 20132436, 화합물수율 46%

시약·촉매·용매 2

HCID 887Methanol용매HCID 14797Potassium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ed3e99f54e074df78f952d9645a28d95
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04757074

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