Triethylamine → N-(1-cyclopropyl piperidine-4-carbonyl)-N'-(5-amino-6-chloro chroman-8-carbonyl) hydrazine

HRID 1523730

반응식

HRID 1523730 반응식
[NH2:1][C:2]1[C:11]([Cl:12])=[CH:10][C:9]([C:13]([NH:15][NH2:16])=[O:14])=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][O:7]2.C(N(CC)CC)C.[CH:24]1([N:27]2[CH2:32][CH2:31][CH:30]([C:33](Cl)=[O:34])[CH2:29][CH2:28]2)[CH2:26][CH2:25]1>ClCCl.O>[CH:24]1([N:27]2[CH2:28][CH2:29][CH:30]([C:33]([NH:16][NH:15][C:13]([C:9]3[CH:10]=[C:11]([Cl:12])[C:2]([NH2:1])=[C:3]4[C:8]=3[O:7][CH2:6][CH2:5][CH2:4]4)=[O:14])=[O:34])[CH2:31][CH2:32]2)[CH2:26][CH2:25]1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 867249091-Cyclopropylpiperidine-4-carbonyl chlorideHCID 867249165-Amino-6-chloro-chroman-8-carboxylic acid hydrazide

생성물 1

HCID 86724915N-(1-cyclopropyl piperidine-4-carbonyl)-N'-(5-amino-6-chloro chroman-8-carbonyl) hydrazine수율 81%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of 5-amino-6-chloro chroman-8-carboxylic acid hydrazide (8.0 grams, 33.1 mmol, obtained in preparation 1) in dichloromethane (200 mL) cooled at 0° C., was added triethylamine (13.9 mL, 99.9 mmol) and a solution of 1-cyclopropylpiperidine-4-carbonyl chloride (11.0 grams) in dichloromethane (200 mL). The reaction mixture was warmed to room temperature and stirred for 16 hours before diluting it with water (160 mL). The two layers were separated, the organic layer was dried over anhydrous sodium sulphate and the volatiles were removed under reduced pressure to obtain the title compound (10.5 grams).

후처리

  1. customThe two layers were separated
  2. dry with materialthe organic layer was dried over anhydrous sodium sulphate
  3. customthe volatiles were removed under reduced pressure

출처 및 근거

ORD 기록
ord-3bdfdfdec219413d9b0eec5a5bcc5a1d
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079894B2

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