Phosgene → HCID 59863032、化合物

HRID 2064066ノート

反応式

HRID 2064066 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1.[C:23](Cl)(Cl)=[O:24].C(N(CC)CC)C>ClCCl>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:23](=[O:24])[N:9]([CH:10]3[CH2:11][CH2:12][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:14][CH2:15]3)[C:3]=2[CH:4]=1

参加物

5

反応物 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 57423910HCID 57423910、化合物

生成物 1

HCID 59863032HCID 59863032、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

1,1-Dimethylethyl 4-[(2-amino-5-chlorophenyl)amino]-1-piperidinecarboxylate (D28) (5.8 g) was dissolved in 100 ml of dichloromethane at 0° C. and phosgene (20% in toluene, 10 ml) and triethylamine (5.6 ml) were added and the mixture was stirred at 0° C. for 1 h, then washed with aqueous citric acid, dried over MgSO4, filtered and evaporated The product was crystallised from diethyl ether to yield the title compound, 5.7 g.

後処理

  1. washwashed with aqueous citric acid
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customevaporated The product
  5. customwas crystallised from diethyl ether

出典と根拠

ORDレコード
ord-78cc5d8a778a4467839a0aed8a6e065e
出典データセット
uspto-grants-2012_10
特許番号
US08288413B2

反応ノート

読み込み中…