Methylamine → HCID 54965987, 화합물

HRID 1429661노트

반응식

HRID 1429661 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[CH2:5][N:6]1[CH2:11][CH2:10][C:9](=O)[CH2:8][CH2:7]1.S1C=CC=C1.[CH3:22][NH2:23].[H][H]>[Pd].CO>[F:1][C:2]1[CH:3]=[C:4]([CH:13]=[CH:14][C:15]=1[F:16])[CH2:5][N:6]1[CH2:11][CH2:10][CH:9]([NH:23][CH3:22])[CH2:8][CH2:7]1

참가 물질

7

반응물 4

HCID 6329MethylamineHCID 8030ThiopheneHCID 23218604HCID 23218604, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 54965987HCID 54965987, 화합물수율 81%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A suspension of D4 (5.4 g, 24 mmol), thiophene solution (4% in diisopropylether; 2 ml), methylamine solution (40% in water, 10 ml) and 10% palladium on carbon (2 g) in methanol (150 ml) were hydrogenated at atmospheric pressure and temperature until 1 eq. (˜600 ml) of hydrogen had been taken up. After this period, the reaction mixture was filtered and the filtrate evaporated in vacuo. The crude product was purified by column chromatography (silica; 5%-10% ammonia in methanol/dichloromethane) to give D5 (4.7 g, 81%). C13H18F2N2 requires 240; Found 241 (MH+)

후처리

  1. waitAfter this period
  2. filtrationthe reaction mixture was filtered
  3. customthe filtrate evaporated in vacuo
  4. customThe crude product was purified by column chromatography (silica; 5%-10% ammonia in methanol/dichloromethane)

출처 및 근거

ORD 기록
ord-8fafb6609754459aa8e53b8264098888
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08940743B2

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