Water → HCID 5282563, 화합물

HRID 379580노트

반응식

HRID 379580 반응식
[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]

참가 물질

6

반응물 4

HCID 962WaterHCID 516892Sodium BicarbonateHCID 4311764Sodium borohydride2회HCID 52825623,4-Diethyl 2-aMinothiophene-3,4-dicarboxylate

생성물 1

HCID 5282563HCID 5282563, 화합물수율 172.4%

시약·촉매·용매 1

HCID 6590Isobutyric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-95cb73f5693144e38dd0ae18fd3a6c07
출처 데이터셋
uspto-grants-2001_10
특허 번호
US06300334B1

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