Water → HCID 136346629, 화합물

HRID 556358노트

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HRID 556358 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]3[C:22]4[CH:23]=[CH:24][C:25]([O:27]C)=[CH:26][C:21]=4[S:20][N:19]=3)=[O:17])=[CH:11][C:10]=2[C:29]([F:32])([F:31])[F:30])[CH2:4][CH2:3]1.B(Br)(Br)Br.O.C([O-])([O-])=O.[Na+].[Na+]>C(Cl)Cl.CCOC(C)=O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([CH2:8][C:9]2[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]3[C:22]4[CH:23]=[CH:24][C:25]([OH:27])=[CH:26][C:21]=4[S:20][N:19]=3)=[O:17])=[CH:11][C:10]=2[C:29]([F:32])([F:30])[F:31])[CH2:4][CH2:3]1

참가 물질

7

반응물 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 25134Boron tribromideHCID 669928876-Methoxy-benzo[d]isothiazole-3-carboxylic acid [4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethyl-phenyl]-amide

생성물 1

HCID 136346629HCID 136346629, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

1.923 g (4.14 mMol) 6-methoxy-benzo[d]isothiazole-3-carboxylic acid [4-(4-methyl-piperazin-1-ylmethyl)-3-trifluoromethyl-phenyl]-amide in 120 ml of a 1 M solution of BBr3 in CH2Cl2 are stirred for 16 h at 45° C. Then the solution is poured into water and EtOAc, the aq. layer is neutralized with Na2CO3, separated off and extracted twice with EtOAc. The organic layers are washed twice with water and brine, dried (Na2SO4) and concentrated. Reversed phase chromatography (Gilson system) gives the title compound: MS: [M−1]=451; HPLC: tRet=11.6.

후처리

  1. customseparated off
  2. extractionextracted twice with EtOAc
  3. washThe organic layers are washed twice with water and brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-1f714be5457542928f0e0284de6a2e20
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058276B2

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