2-Aminopyridine → HCID 178522124、化合物

HRID 623293

反応式

HRID 623293 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][N:3]=1.CCN=C=NCCCN(C)C.Cl.[Cl:20][C:21]([F:26])([F:25])[C:22](O)=[O:23]>ClCCl.CN(C1C=CN=CC=1)C>[Cl:20][C:21]([F:26])([F:25])[C:22]([N:1]=[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][NH:3]1)=[O:23]

参加物

6

反応物 3

HCID 104392-AminopyridineHCID 66154Chlorodifluoroacetic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 178522124HCID 178522124、化合物収率 24%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒2 回

実験手順

200 mg (2.13 mmol) of 2-aminopyridine was dissolved in 5 ml of dichloromethane, 491 mg (2.55 mmol) of EDC-HCl, 311 mg (2.55 mmol) of DMAP and 187 μl (2.23 mmol, 290 mg) of chlorodifluoroacetic acid were added thereto in sequence, and the resulting mixture was stirred overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed with water and 1% hydrochloric acid, and then dried over anhydrous magnesium sulfate to obtain 105 mg (yield 24%) of 2-chloro-2,2-difluoro-N-(pyridin-2(1H)-ylidene)acetamide.

後処理

  1. washwashed with water and 1% hydrochloric acid
  2. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-257a8f432d0c4ef5aa005a2342a2e2f5
出典データセット
uspto-grants-2016_04
特許番号
US09301525B2

関連ノート

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