Aluminium lithium hydride → (3-(2-Amino-4-chlorophenoxy)cyclopentyl)methanol

HRID 1773587노트

반응식

HRID 1773587 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C([O:9][C:10]([CH:12]1[CH2:16][CH2:15][CH:14]([O:17][C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][C:19]=2[NH2:25])[CH2:13]1)=O)C>O1CCCC1>[NH2:25][C:19]1[CH:20]=[C:21]([Cl:24])[CH:22]=[CH:23][C:18]=1[O:17][CH:14]1[CH2:15][CH2:16][CH:12]([CH2:10][OH:9])[CH2:13]1

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 580563063-(2-Amino-4-chloro-phenoxy)-cyclopentanecarboxylic acid ethyl ester

생성물 1

HCID 58056289(3-(2-Amino-4-chlorophenoxy)cyclopentyl)methanol수율 105.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of lithium aluminum hydride (1 M, 3 mL) was added to a cooled (0° C.) solution of 3-(2-amino-4-chloro-phenoxy)-cyclopentanecarboxylic acid ethyl ester (0.2 g) in tetrahydrofuran (5 mL) and the resulting mixture was stirred for 30 minutes. The reaction mixture was then quenched by addition of a saturated aqueous solution of ammonium chloride and filtered. The filter cake was washed with ethyl acetate and the filtrate was dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure to give 180 mg of [3-(2-amino-4-chloro-phenoxy)-cyclopentyl]-methanol without further purifications.

후처리

  1. customThe reaction mixture was then quenched by addition of a saturated aqueous solution of ammonium chloride
  2. filtrationfiltered
  3. washThe filter cake was washed with ethyl acetate
  4. dry with materialthe filtrate was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-57337be362c24a35964933c1418d25a5
출처 데이터셋
uspto-grants-2016_02
특허 번호
US09255110B2

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