Water → HCID 136346629、化合物

HRID 556358ノート

反応式

HRID 556358 の反応式
[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

参加物

7

反応物 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

生成物 1

HCID 136346629HCID 136346629、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f714be5457542928f0e0284de6a2e20
出典データセット
uspto-grants-2011_11
特許番号
US08058276B2

反応ノート

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