1-(4-Fluorophenyl)piperazine → 2-[3-[4-(4-fluorophenyl)-1-piperazinyl]propyl]-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one

HRID 235628ノート

反応式

HRID 235628 の反応式
Br[CH2:2][CH2:3][CH2:4][CH:5]1[C:10](=[O:11])[NH:9][C:8]2[CH:12]=[C:13]([CH3:17])[C:14]([CH3:16])=[CH:15][C:7]=2[S:6]1.[F:18][C:19]1[CH:24]=[CH:23][C:22]([N:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[CH:21][CH:20]=1>C(OCC)(=O)C>[F:18][C:19]1[CH:20]=[CH:21][C:22]([N:25]2[CH2:30][CH2:29][N:28]([CH2:2][CH2:3][CH2:4][CH:5]3[C:10](=[O:11])[NH:9][C:8]4[CH:12]=[C:13]([CH3:17])[C:14]([CH3:16])=[CH:15][C:7]=4[S:6]3)[CH2:27][CH2:26]2)=[CH:23][CH:24]=1

参加物

4

反応物 2

HCID 752601-(4-Fluorophenyl)piperazineHCID 137846132-(3-bromopropyl)-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one

生成物 1

HCID 137846402-[3-[4-(4-fluorophenyl)-1-piperazinyl]propyl]-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one収率 78.6%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
110 °C

実験手順

In 10 ml of ethyl acetate were dissolved 628 mg of 2-(3-bromopropyl)-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one and 721 mg of 1-(4-fluorophenyl)piperazine. The solution was concentrated and the concentrate was stirred at 110° C. for one hour, diluted with water, and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried over MgSO4 and concentrated to give 2-[3-[4-(4-fluorophenyl)-1-piperazinyl]propyl]-6,7-dimethyl-2H-1,4-benzothiazin-3(4H)-one (650 mg, 78.6%). Recrystallization from methanol gave colorless prisms, m.p. 161°-162° C.

後処理

  1. concentrationThe solution was concentrated
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-00d3682dc3a84113a1e9543fe0a112b5
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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