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

HRID 1523730ノート

反応式

HRID 1523730 の反応式
[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

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3bdfdfdec219413d9b0eec5a5bcc5a1d
出典データセット
uspto-grants-2015_07
特許番号
US09079894B2

反応ノート

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