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

HRID 1064597ノート

反応式

HRID 1064597 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
80 °C

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-0ce68225d99a411dbfe29fac8889b329
出典データセット
uspto-grants-2005_11
特許番号
US06969713B2

反応ノート

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