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

HRID 235628노트

반응식

HRID 235628 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00d3682dc3a84113a1e9543fe0a112b5
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04640916

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