Acetic Anhydride → HCID 68855307, 화합물

HRID 1818703노트

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HRID 1818703 반응식
[NH2:1][CH:2]([CH2:17][O:18][C:19]1[CH:20]=[CH:21][C:22]2[S:26][C:25]([CH3:27])=[N:24][C:23]=2[CH:28]=1)[CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1.[C:29](OC(=O)C)(=[O:31])[CH3:30]>CN(C)C1C=CN=CC=1.C(Cl)Cl.C(N(CC)CC)C>[C:29]([NH:1][CH:2]([CH2:17][O:18][C:19]1[CH:20]=[CH:21][C:22]2[S:26][C:25]([CH3:27])=[N:24][C:23]=2[CH:28]=1)[CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1)(=[O:31])[CH3:30]

참가 물질

6

반응물 2

HCID 7918Acetic AnhydrideHCID 68855493HCID 68855493, 화합물

생성물 1

HCID 68855307HCID 68855307, 화합물

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a solution of tert-butyl 4-[2-amino-3-(2-methylbenzothiazol-5-yloxy)propyl]-piperazinecarboxylate (260 mg) and 4-dimethylaminopyridine (3 mg) in methylene chloride (6 ml) and triethylamine (178 μl) at 0° C. was added acetic anhydride (160 mg), and the mixture allowed to warm to room temperature. After stirring overnight, the mixture was partitioned between methylene chloride and water, and solvent removed from the organic layer under reduced pressure. The residue was chromatographed on a silica gel column, eluting with 25% ethyl acetate/hexanes followed by 10% methanol/methylene chloride, to provide crude tert-butyl 4-[2-(acetylamino)-3-(2-methylbenzothiazol-5-yloxy)propyl]piperazinecarboxylate, which was purified by preparative TLC.

후처리

  1. customthe mixture was partitioned between methylene chloride and water, and solvent
  2. customremoved from the organic layer under reduced pressure
  3. customThe residue was chromatographed on a silica gel column
  4. washeluting with 25% ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-e0d5aa54988f4409b8902449f454ea9e
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07601721B2

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