1-Chloroethyl chloroformate → cis-1-(3-Cyanobenzenesulphonyl)-2,6-dimethylpiperazine

HRID 1064597노트

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HRID 1064597 반응식
[C:1]([C:3]1[CH:4]=[C:5]([S:9]([N:12]2[C@H:17]([CH3:18])[CH2:16][N:15](CC3C=CC=CC=3)[CH2:14][C@@H:13]2[CH3:26])(=[O:11])=[O:10])[CH:6]=[CH:7][CH:8]=1)#[N:2].ClC(OC(Cl)C)=O>ClCCCl>[C:1]([C:3]1[CH:4]=[C:5]([S:9]([N:12]2[C@H:17]([CH3:18])[CH2:16][NH:15][CH2:14][C@@H:13]2[CH3:26])(=[O:10])=[O:11])[CH:6]=[CH:7][CH:8]=1)#[N:2]

참가 물질

4

반응물 2

HCID 5213051-Chloroethyl chloroformateHCID 69746861cis-1-(3-Cyanobenzenesulphonyl)-2,6-dimethyl-4-phenylmethylpiperazine

생성물 1

HCID 69744750cis-1-(3-Cyanobenzenesulphonyl)-2,6-dimethylpiperazine

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
80 °C

실험 절차

A solution of the product from step (i) (1 g) in 1,2-dichloroethane (10 ml) was treated with 1-chloroethyl chloroformate (0.44 ml). The mixture was heated at 80° C. for 16 h. The solvents were then evaporated under reduced pressure and the residue dissolved in methanol (50 ml). The mixture then heated at 50° C. for 1 h. The solvents were then evaporated under reduced pressure. Purification was by trituration with ethyl acetate and filtration to give the subtitle compound as a white solid. Yield: 0.85 g

후처리

  1. customThe solvents were then evaporated under reduced pressure
  2. dissolutionthe residue dissolved in methanol (50 ml)
  3. temperatureThe mixture then heated at 50° C. for 1 h
  4. customThe solvents were then evaporated under reduced pressure
  5. customPurification
  6. filtrationwas by trituration with ethyl acetate and filtration

출처 및 근거

ORD 기록
ord-0ce68225d99a411dbfe29fac8889b329
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06969713B2

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