Boron tribromide → HCID 11531195, 화합물

HRID 1766059노트

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HRID 1766059 반응식
[C:1]([NH:5][C:6]([C:8]1[S:26][C:11]2[N:12]=[C:13]([S:24][CH3:25])[N:14]=[C:15]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([O:22]C)[CH:17]=3)[C:10]=2[C:9]=1[NH2:27])=[O:7])([CH3:4])([CH3:3])[CH3:2].B(Br)(Br)Br.C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:1]([NH:5][C:6]([C:8]1[S:26][C:11]2[N:12]=[C:13]([S:24][CH3:25])[N:14]=[C:15]([C:16]3[CH:21]=[CH:20][CH:19]=[C:18]([OH:22])[CH:17]=3)[C:10]=2[C:9]=1[NH2:27])=[O:7])([CH3:4])([CH3:2])[CH3:3]

참가 물질

5

반응물 3

HCID 25134Boron tribromideHCID 516892Sodium BicarbonateHCID 9887381Org-41841

생성물 1

HCID 11531195HCID 11531195, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

tert-Butyl 5-amino-2-methylthio-4-(3-methoxyphenyl)-thieno[2,3-d]pyrimidine-6-carboxamide (example 1e, 1.8 g) was dissolved in dry CH2Cl2 (30 ml) and the resulting solution was cooled down to 0° C. A solution of boron tribromide (1.28 ml) in dry CH2Cl2 (30 ml) was added dropwise and the mixture was stirred overnight at room temperature. Sat. aq. NaHCO3 was added dropwise to the reaction mixture until cessation of the exothermic reaction. Thereafter, CH2Cl2 was removed from the mixture by evaporation and a large amount of EtOAc was added. The organic layer was washed with sat. aq. NaHCO3, dried (MgSO4) and concentrated in vacuo.

후처리

  1. customThereafter, CH2Cl2 was removed from the mixture by evaporation
  2. additiona large amount of EtOAc was added
  3. washThe organic layer was washed with sat. aq. NaHCO3
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-a7911500208f46019c1557b1841c299a
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07229990B2

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