Potassium Carbonate → Ethyl4-(1-(3,4-Difluorobenzylamino)-4,4-dimethyl-1,3-dioxopentan-2-yl)-3-nitrobenzoate

HRID 40113

반응식

HRID 40113 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:16]=[CH:17][C:18]=1[F:19])[CH2:5][NH:6][C:7](=[O:15])[CH2:8][C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11].[CH2:20]([O:22][C:23](=[O:34])[C:24]1[CH:29]=[CH:28][C:27](F)=[C:26]([N+:31]([O-:33])=[O:32])[CH:25]=1)[CH3:21].C([O-])([O-])=O.[K+].[K+]>CS(C)=O.CCOC(C)=O>[F:1][C:2]1[CH:3]=[C:4]([CH:16]=[CH:17][C:18]=1[F:19])[CH2:5][NH:6][C:7](=[O:15])[CH:8]([C:27]1[CH:28]=[CH:29][C:24]([C:23]([O:22][CH2:20][CH3:21])=[O:34])=[CH:25][C:26]=1[N+:31]([O-:33])=[O:32])[C:9](=[O:14])[C:10]([CH3:13])([CH3:12])[CH3:11]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 21277355Ethyl 4-fluoro-3-nitrobenzoate2회HCID 59762316HCID 59762316, 화합물2회

생성물 1

HCID 59762433Ethyl4-(1-(3,4-Difluorobenzylamino)-4,4-dimethyl-1,3-dioxopentan-2-yl)-3-nitrobenzoate

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of N-(3,4-difluorobenzyl)-4,4-dimethyl-3-oxopentanamide (Compound 112, 126 mg, 0.47 mmol) and ethyl4-fluoro-3-nitrobenzoate (Compound 113, 100 mg, 0.47 mmol) in DMSO (1 ml) was added K2CO3 (130 mg, 0.94 mmol). The mixture was stirred at room temperature for 16 h, diluted with EtOAc, washed with 1 M HCl, H2O, and brine, dried over Na2SO4, and concentrated in vacuo. The residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes) to yield the title compound as a yellow solid.

후처리

  1. washwashed with 1 M HCl, H2O, and brine
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography on silica gel (0→30% EtOAc-hexanes)

출처 및 근거

ORD 기록
ord-458a7423207f404ebdf8a47f33f1bb6e
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524917B2

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