1,2-Dichloroethane → (5-Chlorocarbonyl-pyridin-2-yl)-methyl-carbamic acid tert-butyl ester

HRID 595089ノート

反応式

HRID 595089 の反応式
[C:1]([O:5][C:6]([N:8]([CH3:18])[C:9]1[CH:17]=[CH:16][C:12]([C:13](O)=[O:14])=[CH:11][N:10]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CN.[Cl:21]CCCl>>[C:1]([O:5][C:6](=[O:7])[N:8]([C:9]1[CH:17]=[CH:16][C:12]([C:13]([Cl:21])=[O:14])=[CH:11][N:10]=1)[CH3:18])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 3

HCID 111,2-DichloroethaneHCID 6329MethylamineHCID 667695966-((tert-Butoxycarbonyl)(methyl)amino)nicotinic acid

生成物 1

HCID 86664608(5-Chlorocarbonyl-pyridin-2-yl)-methyl-carbamic acid tert-butyl ester

実験手順

6-(tert-Butoxycarbonyl-methyl-amino)-nicotinic acid (12.5 g, 47.0 mmol) (prepared analogously to A-08 using methyl amine instead of ethylamine) is taken up in 300 mL DCE, 1-chloro-N,N-2-trimethylpropenyl-amine (10.0 mL, 74.8 mmol) is added and the reaction mixture is stirred overnight at RT. The reaction mixture is concentrated under reduced pressure and the crude product is used in the next step without purification.

後処理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. customthe crude product is used in the next step without purification

出典と根拠

ORDレコード
ord-bf3d18c3d7cf4427a65888a6a7e7691e
出典データセット
uspto-grants-2016_01
特許番号
US09243000B2

反応ノート

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