2-Amino-5-methoxybenzene-1-thiol → 2-(2-bromoethyl)-7-methoxy-2H-1,4-benzothiazin-3(4H)-one

HRID 235637ノート

反応式

HRID 235637 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[SH:10].Br[CH:12]([CH2:17][CH2:18][Br:19])[C:13](OC)=[O:14]>CN(C)C=O>[Br:19][CH2:18][CH2:17][CH:12]1[C:13](=[O:14])[NH:1][C:2]2[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=2[S:10]1

参加物

4

反応物 2

HCID 2355092-Amino-5-methoxybenzene-1-thiolHCID 296716Methyl 2,4-dibromobutanoate

生成物 1

HCID 137846242-(2-bromoethyl)-7-methoxy-2H-1,4-benzothiazin-3(4H)-one収率 65.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3.10 g of 2-amino-5-methoxythiophenol and 5.20 g of methyl 2,4-dibromobutyrate in 30 ml of dimethylformamide was stirred at room temperature for 2 hours. The mixture was poured into ice-water and the resulting crystals were collected by filtration and washed with water. Recrystallization from methanol gave 3.94 g (65.2%) of 2-(2-bromoethyl)-7-methoxy-2H-1,4-benzothiazin-3(4H)-one as prisms, m.p. 142°-143° C.

後処理

  1. filtrationthe resulting crystals were collected by filtration
  2. washwashed with water
  3. customRecrystallization from methanol

出典と根拠

ORDレコード
ord-4128f83a82374103b87f503118da9ba2
出典データセット
uspto-grants-1987_02
特許番号
US04640916

反応ノート

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