Acetic Anhydride → HCID 57439883, 화합물

HRID 906036노트

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HRID 906036 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 57439883HCID 57439883, 화합물수율 90%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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)+

후처리

  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

출처 및 근거

ORD 기록
ord-744a580611014449bdbdc175e2c4a140
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08012982B2

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