4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid methyl ester → 4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid

HRID 641485노트

반응식

HRID 641485 반응식
C[O:2][C:3](=[O:28])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:27]=[CH:26][C:15]3[CH2:16][CH2:17][N:18]([CH:21]4[CH2:25][CH2:24][CH2:23][CH2:22]4)[CH2:19][CH2:20][C:14]=3[CH:13]=2)=[CH:6][CH:5]=1>CO.[OH-].[Na+].O>[CH:21]1([N:18]2[CH2:19][CH2:20][C:14]3[CH:13]=[C:12]([O:11][CH2:10][C:7]4[CH:8]=[CH:9][C:4]([C:3]([OH:28])=[O:2])=[CH:5][CH:6]=4)[CH:27]=[CH:26][C:15]=3[CH2:16][CH2:17]2)[CH2:22][CH2:23][CH2:24][CH2:25]1

참가 물질

5

반응물 1

HCID 104523174-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid methyl ester

생성물 1

HCID 103614874-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 14798Sodium Hydroxide용매

반응 조건

온도
60 °C

실험 절차

4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxymethyl)-benzoic acid methyl ester (E88) (3.1 g, 8.1 mmol)) was dissolved in a mixture of methanol (90 ml), 2N sodium hydroxide (12 ml) and water (30 ml). The resulting mixture was stirred at 60° C. for 4 hours and then cooled to room temperature. The mixture was concentrated in vacuo to remove the organic solvents and then acidified to pH 6 (2N hydrochloric acid). The resulting precipitates were filtered, washed with water and dried under vacuum to afford the title compound (E89); MS (ES+) m/e 366 [M+H]+.

후처리

  1. temperaturecooled to room temperature
  2. concentrationThe mixture was concentrated in vacuo
  3. customto remove the organic solvents
  4. customThe resulting precipitates
  5. filtrationwere filtered
  6. washwashed with water
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-61e4c0836feb4033bbee85b3c304a93b
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07696193B2

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