Methanol → HCID 59635786, 화합물

HRID 1187946노트

반응식

HRID 1187946 반응식
[BH4-].[Li+].C[O:4][C:5](=O)[C:6]([CH3:17])([CH3:16])[CH2:7][N:8]1[CH:13]=[CH:12][C:11]([Br:14])=[CH:10][C:9]1=[O:15].CO>O1CCCC1.[O-]S([O-])(=O)=O.[Mg+2]>[Br:14][C:11]1[CH:12]=[CH:13][N:8]([CH2:7][C:6]([CH3:16])([CH3:17])[CH2:5][OH:4])[C:9](=[O:15])[CH:10]=1

참가 물질

6

반응물 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 59635660HCID 59635660, 화합물

생성물 1

HCID 59635786HCID 59635786, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 24083Sulfuric acid magnesium salt (1:1)용매

실험 절차

Lithium borohydride (25 mg) was added to a solution of 3-(4-bromo-2-oxo-2H-pyridin-1-yl)-2,2-dimethyl-propionic acid methyl ester (0.29 g) in tetrahydrofuran (3 mL) chilled in an ice bath. Then methanol (45 μL) was added and the mixture was stirred in the cooling bath for 1 h and at room temperature overnight. The mixture was diluted with tetrahydrofuran and MgSO4 was added. The mixture was filtered and the filtrate was concentrated. The residue was purified by chromatography on silica gel (cyclohexane/ethyl acetate 1:1) to afford the title compound as a colorless oil. Yield: 0.13 g (49% of theory); Mass spectrum (ESI+): m/z=260/262 (Br) [M+H]+.

후처리

  1. temperaturechilled in an ice bath
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. customThe residue was purified by chromatography on silica gel (cyclohexane/ethyl acetate 1:1)

출처 및 근거

ORD 기록
ord-498fb0312377493b8312c3b50fd4167e
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08673899B2

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