Sodium Bicarbonate → HCID 66736620, 화합물

HRID 1803860노트

반응식

HRID 1803860 반응식
[C:1]([O:5][C:6](=[O:15])[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1F)([CH3:4])([CH3:3])[CH3:2].C([O-])(O)=O.[Na+].[CH3:21][O:22][CH2:23][C@H:24]([NH2:26])[CH3:25]>>[C:1]([O:5][C:6](=[O:15])[C:7]1[CH:12]=[CH:11][C:10]([F:13])=[CH:9][C:8]=1[NH:26][C@H:24]([CH3:25])[CH2:23][O:22][CH3:21])([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 3

HCID 516892Sodium BicarbonateHCID 10313069(+)-2-Amino-1-methoxypropaneHCID 57447335Tert-butyl 2,4-difluorobenzoate

생성물 1

HCID 66736620HCID 66736620, 화합물수율 84%

반응 조건

온도
65 °C

실험 절차

A mixture of 2,4-difluoro-benzoic acid tert-butyl ester (30 g, 140.05 mmol) and (R)-2-methoxy-1-methyl-ethylamine (100 mL) was stirred at 65° C. for 2 days. A satured solution of NaHCO3 was added and the mixture was extracted with dichloromethane (3 times). The organic phase was washed twice with water then with brine, dried over sodium sulfate filtered and evaporated to dryness to obtain a crude, which was purified by column chromatography on silica gel (exane/ethyl acetate 9:1). The title compound (33.38 g, 84%) was obtained as oil.

후처리

  1. extractionthe mixture was extracted with dichloromethane (3 times)
  2. washThe organic phase was washed twice with water
  3. dry with materialwith brine, dried over sodium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customto obtain a crude, which
  7. customwas purified by column chromatography on silica gel (exane/ethyl acetate 9:1)

출처 및 근거

ORD 기록
ord-40229a2380e64255b36865ac1950572d
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354399B2

반응 노트

불러오는 중…