Water → HCID 5282563、化合物

HRID 379580ノート

反応式

HRID 379580 の反応式
[BH4-].[Na+].[NH2:3][C:4]1[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].O.C(=O)(O)[O-].[Na+]>C(O)(=O)C(C)C>[CH3:6][CH:7]([CH3:14])[CH2:8][NH:3][C:4]1[S:5][CH:6]=[C:7]([C:14]([O:16][CH2:17][CH3:18])=[O:15])[C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

参加物

6

反応物 4

HCID 962WaterHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydride2 回HCID 52825623,4-Diethyl 2-aMinothiophene-3,4-dicarboxylate

生成物 1

HCID 5282563HCID 5282563、化合物収率 172.4%

試薬・触媒・溶媒 1

HCID 6590Isobutyric Acid溶媒

実験手順

Sodium borohydride (18 g) was added portionwise over 5 hours to a stirred suspension of diethyl 2-aminothiophene-3,4-dicarboxyate (33 g) in isobutyric acid (300 ml) at room temperature. The mixture was stirred for 16 hours then further sodium borohydride (4 g) was added and stirring was continued for 5 hours. Water (1.51) was added, the mixture was neutralised by addition of solid sodium bicarbonate and then extracted with ether (3×500 ml). The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated to give the subtitle compound (35 g) as a solid.

後処理

  1. stirringstirring
  2. waitwas continued for 5 hours
  3. extractionextracted with ether (3×500 ml)
  4. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated

出典と根拠

ORDレコード
ord-95cb73f5693144e38dd0ae18fd3a6c07
出典データセット
uspto-grants-2001_10
特許番号
US06300334B1

反応ノート

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