Acetic Anhydride → HCID 57439883、化合物

HRID 906036ノート

反応式

HRID 906036 の反応式
[CH3:1]CN(CC)CC.[CH3:8][C:9]([O:11][C:12]([CH3:14])=[O:13])=O.OC1C=[CH:20][C:19]([NH:22][C:23]([C:25]2[CH:30]=[CH:29][C:28]([N:31]3[CH2:36][CH2:35][N:34]([C:37]([O:39][C:40]([CH3:43])([CH3:42])[CH3:41])=[O:38])[CH2:33][CH2:32]3)=[CH:27][CH:26]=2)=O)=[CH:18][CH:17]=1>C(Cl)Cl>[C:12]([O:11][C:9]1[CH:17]=[CH:18][C:19]([NH:22][C:23]([C:25]2[CH:30]=[CH:29][C:28]([N:31]3[CH2:32][CH2:33][N:34]([C:37]([O:39][C:40]([CH3:41])([CH3:43])[CH3:42])=[O:38])[CH2:35][CH2:36]3)=[CH:27][CH:26]=2)=[CH2:1])=[CH:20][CH:8]=1)(=[O:13])[CH3:14]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 11516825Tert-butyl 4-[4-[(4-hydroxyphenyl)carbamoyl]phenyl]piperazine-1-carboxylate

生成物 1

HCID 57439883HCID 57439883、化合物収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

1.1 eq of Et3N and 2 eq of Ac2O were added to a solution of tert-butyl 4-(4-{[(4-hydroxyphenyl)amino]carbonyl}phenyl)piperazine-1-carboxylate in dry DCM (0.1 M) (prepared as described in published International patent application WO98/00134) and the solution stirred at RT for 16 h under a nitrogen atmosphere. The reaction mixture was diluted with DCM and the organic phase was washed with aqueous HCl (1N) (twice), saturated aqueous NaHCO3 and then brine. The organic phase was dried over Na2SO4, filtered and the solvent evaporated in vacuo to afford the title compound as a white solid (90%); MS (ES+) m/z 440 (M+H)+

後処理

  1. washthe organic phase was washed with aqueous HCl (1N) (twice), saturated aqueous NaHCO3
  2. dry with materialThe organic phase was dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-744a580611014449bdbdc175e2c4a140
出典データセット
uspto-grants-2011_09
特許番号
US08012982B2

反応ノート

読み込み中…