Boron tribromide → HCID 22119820、化合物

HRID 1274645ノート

反応式

HRID 1274645 の反応式
[CH3:1][N:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([C:21]([CH3:28])([CH3:27])[C:22]([O:24]CC)=[O:23])[C:17]=3[CH:29]=2)[C:3]1=[O:30].B(Br)(Br)Br>C(Cl)Cl>[CH3:1][N:2]1[C:7]([C:8]([F:9])([F:10])[F:11])=[CH:6][C:5](=[O:12])[N:4]([C:13]2[CH:14]=[CH:15][C:16]3[S:20][N:19]=[C:18]([C:21]([CH3:27])([CH3:28])[C:22]([OH:24])=[O:23])[C:17]=3[CH:29]=2)[C:3]1=[O:30]

参加物

4

反応物 2

HCID 25134Boron tribromideHCID 18314487HCID 18314487、化合物

生成物 1

HCID 22119820HCID 22119820、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of ethyl 5-[3,6-dihydro-3-methyl-2,6-dioxo-4-(trifluoromethyl)-1(2H)-pyrimidinyl]-α,α-dimethyl-1,2-benzisothiazole-3-acetate (6.30 g, 0.0143 mol) in methylene chloride at 0° C. is added boron tribromide in methylene chloride (1.0 M, 100 ml, 0.100 mol) such that the temperature does not exceed 15° C. The resultant mixture is stirred one hour at ambient temperature, quenched with 3 N hydrochloric acid, and diluted with methylene chloride. The organic layer is separated, washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title compound as an off-white solid (mp 155-156° C.) which is identified by NMR and IR spectral analyses.

後処理

  1. customdoes not exceed 15° C
  2. customquenched with 3 N hydrochloric acid
  3. additiondiluted with methylene chloride
  4. customThe organic layer is separated
  5. washwashed sequentially with water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-17166df07975465cab2acb562b0ccce3
出典データセット
uspto-grants-2000_12
特許番号
US06156700

反応ノート

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