Phosgeniminium chloride → HCID 73852578、化合物

HRID 719502ノート

反応式

HRID 719502 の反応式
[NH2:1][C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:9][CH:8]=2)[N:5]=[CH:4][C:3]=1[C:17]#[N:18].[CH3:19][N+:20]([CH3:24])=[C:21](Cl)[Cl:22].[Cl-]>ClCCCl>[Cl:22][C:21]([N:20]([CH3:24])[CH3:19])=[N:1][C:2]1[N:6]([C:7]2[CH:8]=[CH:9][C:10]([S:13]([CH3:16])(=[O:15])=[O:14])=[CH:11][CH:12]=2)[N:5]=[CH:4][C:3]=1[C:17]#[N:18]

参加物

4

反応物 2

HCID 2723945Phosgeniminium chlorideHCID 217925045-Amino-1-(4-(methylsulfonyl)phenyl)-1H-pyrazole-4-carbonitrile

生成物 1

HCID 73852578HCID 73852578、化合物収率 80.9%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A solution of 5-amino-1-(4-methanesulfonyl-phenyl)-1H-pyrazole-4-carbonitrile (1.2 g, 4.57 mmol) and phosgeniminium chloride (0.900 g, 7.08 mmol) in dry 1,2-dichloroethane was refluxed for 4 h. The solvent was removed under reduced pressure and the residue was purified by flash chromatography (30 to 50% ethyl acetate/hexanes) to yield 1-chloro-N′-[4-cyano-2-(4-methanesulfonyl-phenyl)-2H-pyrazol-3-yl]-N,N-dimethyl-formamidine (1.3 g, 80%) as a yellowish solid. Exact mass calculated for C14H14ClN5O2S 351.06, found 352.20 (MH+, 100%).

後処理

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was purified by flash chromatography (30 to 50% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-b4370faec47b4ad189d69a31911e63bb
出典データセット
uspto-grants-2006_11
特許番号
US07132426B2

反応ノート

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