Boron tribromide → HCID 22119820, 화합물

HRID 1274645노트

반응식

HRID 1274645 반응식
[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]

참가 물질

4

반응물 2

HCID 25134Boron tribromideHCID 18314487HCID 18314487, 화합물

생성물 1

HCID 22119820HCID 22119820, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-17166df07975465cab2acb562b0ccce3
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06156700

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