Pyridine → HCID 13728618, 화합물

HRID 1365926노트

반응식

HRID 1365926 반응식
ClC(Cl)(OC(=O)[O:6][C:7]([Cl:10])(Cl)Cl)Cl.[N:13]1([C:19](=[O:21])[CH3:20])[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1.N1C=CC=CC=1>C(Cl)Cl>[C:19]([N:13]1[CH2:18][CH2:17][N:16]([C:7]([Cl:10])=[O:6])[CH2:15][CH2:14]1)(=[O:21])[CH3:20]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 837951-AcetylpiperazineHCID 94429Triphosgene

생성물 1

HCID 13728618HCID 13728618, 화합물수율 75.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of carbonic acid ditrichloromethyl ester (triphosgene) (2.31 g, 7.80 mmol) in CH2Cl2 (30 ml) at 0° C., was added a solution of 1-piperazin-1-yl-ethanone (2.0 g, 15.6 mmol) and pyridine (1.38 ml, 17.2 mmol) in CH2Cl2 (5 ml) over 30 minutes. The temperature was raised to RT, and stirring was continued over night. The organic phase was washed with H2O, dried over Na2SO4. Purification by flash chromatography (SiO2, EtOAc) yielded 1.12 g (38%) of the title compound as white solid.

후처리

  1. waitwas continued over night
  2. washThe organic phase was washed with H2O
  3. dry with materialdried over Na2SO4
  4. customPurification by flash chromatography (SiO2, EtOAc)

출처 및 근거

ORD 기록
ord-eb8f9433419340aabce7de6f558a7303
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893062B2

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