Hydrazine hydrate (1:1) → 4-(4-Aminocyclohexyloxy)benzoic acid ethyl ester

HRID 555378노트

반응식

HRID 555378 반응식
[CH2:1]([O:3][C:4](=[O:29])[C:5]1[CH:10]=[CH:9][C:8]([O:11][CH:12]2[CH2:17][CH2:16][CH:15]([N:18]3C(=O)C4C(=CC=CC=4)C3=O)[CH2:14][CH2:13]2)=[CH:7][CH:6]=1)[CH3:2].O.NN>C(Cl)(Cl)Cl.C(O)C>[CH2:1]([O:3][C:4](=[O:29])[C:5]1[CH:6]=[CH:7][C:8]([O:11][CH:12]2[CH2:17][CH2:16][CH:15]([NH2:18])[CH2:14][CH2:13]2)=[CH:9][CH:10]=1)[CH3:2]

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 167566294-[4-(1,3-Dioxo-1,3-dihydro-isoindol-2-yl)-cyclohexyloxy]-benzoic acid ethyl ester

생성물 1

HCID 167561694-(4-Aminocyclohexyloxy)benzoic acid ethyl ester수율 98.5%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6212Chloroform용매

반응 조건

온도
7.5 °C

실험 절차

To a solution of 4-[4-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-cyclohexyloxy]-benzoic acid ethyl ester (6.3 g, 16.0 mmol) in CHCl3 (50 mL) and ethanol (60 mL) was added hydrazine hydrate (16.0 g, 320.2 mmol). Stirring was continued at ambient temperature for 2 days. The reaction mixture was then cooled to 5-10° C. and the white precipitate was filtered off. The filtrate was washed with water, dried and the solvent evaporated under vacuum to afford 4.15 g (98%) of 4-(4-amino-cyclohexyloxy)-benzoic acid ethyl ester.

후처리

  1. filtrationthe white precipitate was filtered off
  2. washThe filtrate was washed with water
  3. customdried
  4. customthe solvent evaporated under vacuum

출처 및 근거

ORD 기록
ord-58ea6859ac654d3c99f40af741ae9cb4
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053447B2

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