Methylamine → HCID 54965987、化合物

HRID 1429661ノート

反応式

HRID 1429661 の反応式
[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

参加物

7

反応物 4

HCID 6329MethylamineHCID 8030ThiopheneHCID 23218604HCID 23218604、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 54965987HCID 54965987、化合物収率 81%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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+)

後処理

  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)

出典と根拠

ORDレコード
ord-8fafb6609754459aa8e53b8264098888
出典データセット
uspto-grants-2015_01
特許番号
US08940743B2

反応ノート

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