Hydrochloric Acid → HCID 66758458、化合物

HRID 1507869ノート

反応式

HRID 1507869 の反応式
[NH2:1][C:2]1[S:3][C:4]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)=[CH:5][C:6]=1[C:7]([O:9]CC)=O.[C:19](#[N:21])[CH3:20].Cl>O1CCOCC1>[F:18][C:15]1[CH:14]=[CH:13][C:12]([C:4]2[S:3][C:2]3[N:1]=[C:19]([CH3:20])[NH:21][C:7](=[O:9])[C:6]=3[CH:5]=2)=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 6342AcetonitrileHCID 21529229Ethyl 2-amino-5-(4-fluorophenyl)thiophene-3-carboxylate

生成物 1

HCID 66758458HCID 66758458、化合物収率 98.6%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of ethyl 2-amino-5-(4-fluorophenyl)thiophene-3-carboxylate (0.3 g, 1.13 mmol) and acetonitrile (0.56 ml, 11.3 mmol) in dioxane (4 ml) was added 4M HCl in dioxane (4 ml). The mixture was stirred at room temperature overnight. The solvents were removed under reduced pressure. The residue was diluted with water and made alcaline with a saturated aqueous sodium bicarbonate solution. The precipitate was filtered off, washed with water and dried. The crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1) to yield the title compound as a white solid (0.29 g, 81%).

後処理

  1. customThe solvents were removed under reduced pressure
  2. additionThe residue was diluted with water
  3. filtrationThe precipitate was filtered off
  4. washwashed with water
  5. customdried
  6. customThe crude residue was purified by flash chromatography on silica gel (CH2Cl2/MeOH 60:1)

出典と根拠

ORDレコード
ord-09aa14ecb4f74aeb908e2d987912a610
出典データセット
uspto-grants-2015_12
特許番号
US09221822B2

反応ノート

読み込み中…