O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamine → HCID 178425979、化合物

HRID 1615630ノート

反応式

HRID 1615630 の反応式
[CH3:1][C:2]1[C:3]([NH2:9])=[N:4][C:5]([CH3:8])=[CH:6][N:7]=1.[C:10]1([CH3:23])[CH:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[C:11]=1[S:18]([O:21][NH2:22])(=[O:20])=[O:19]>C(Cl)Cl>[NH2:22][N:4]1[C:5]([CH3:8])=[CH:6][N:7]=[C:2]([CH3:1])[C:3]1=[NH2+:9].[CH3:17][C:12]1[CH:13]=[C:14]([CH3:16])[CH:15]=[C:10]([CH3:23])[C:11]=1[S:18]([O-:21])(=[O:20])=[O:19]

参加物

4

反応物 2

HCID 11830845O-(2,4,6-Trimethylbenzenesulfonyl)hydroxylamineHCID 132615003,6-Dimethylpyrazin-2-amine

生成物 1

HCID 178425979HCID 178425979、化合物収率 59.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

A mixture of 3,6-dimethylpyrazin-2-amine (1.23 g, 10 mmol) in DCM (20 mL) was cooled to 0° C. and a solution of O-(mesitylsulfonyl)hydroxylamine (4.3 g, 20 mmol) was added slowly. The reaction mixture was allowed to warm to room temperature for 3 h and filtered. The solid collected was washed with DCM (50 mL) to give 1-amino-3,6-dimethylpyrazin-2(1H)-iminium-2,4,6-trimethylbenzenesulfonate as a brown solid (2.0 g, yield 59%). ESI MS: m/z 139 [M-199]+.

後処理

  1. temperatureto warm to room temperature for 3 h
  2. filtrationfiltered
  3. customThe solid collected
  4. washwas washed with DCM (50 mL)

出典と根拠

ORDレコード
ord-7f21115adfec4d91a229d8b0d1d91bc4
出典データセット
uspto-grants-2014_07
特許番号
US08765760B2

反応ノート

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