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Sodium Bicarbonate → ethyl 5-amino-3-methylthiophene-2-carboxylate

HRID 2067315
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HRID 2067315 반응식
Cl.[NH2:2][C:3]1[S:7][C:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([CH3:13])[CH:4]=1.C(=O)(O)[O-].[Na+]>ClCCl>[NH2:2][C:3]1[S:7][C:6]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:5]([CH3:13])[CH:4]=1
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 19100801Ethyl 5-amino-3-methylthiophene-2-carboxylate hydrochloride

생성물 1

HCID 2064026ethyl 5-amino-3-methylthiophene-2-carboxylate수율 98%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Ethyl 5-amino-3-methylthiophene-2-carboxylate hydrochloride (5.80 g, 26.2 mmol) was suspended in dichloromethane (200 mL). To the suspension was added saturated aqueous sodium bicarbonate solution (250 mL). The resulting mixture was stirred for 15 minutes, then the two layers were separated. The aqueous layer was extracted with dichloromethane (100 mL). The combined organic layer was dried over sodium sulphate, filtered and concentrated in vacuo to afford ethyl 5-amino-3-methylthiophene-2-carboxylate (4.75 g, 98%).

후처리

  1. customthe two layers were separated
  2. extractionThe aqueous layer was extracted with dichloromethane (100 mL)
  3. dry with materialThe combined organic layer was dried over sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-bd89e78fa49c4d3380377d3781e175bb
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08293768B2

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