Sodium Bicarbonate → HCID 22258010, 화합물

HRID 1611018노트

반응식

HRID 1611018 반응식
[BH4-].[Na+].[NH2:3][C:4]1[S:5][C:6]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:7][C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10].C(=O)(O)[O-].[Na+]>CC(C)C(O)=O.O>[CH3:4][CH:8]([CH3:9])[CH2:7][NH:3][C:4]1[S:5][C:6]([CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:7][C:8]=1[C:9]([O:11][CH2:12][CH3:13])=[O:10]

참가 물질

6

반응물 3

HCID 516892Sodium BicarbonateHCID 3792137Ethyl 2-amino-5-benzylthiophene-3-carboxylateHCID 4311764Sodium borohydride

생성물 1

HCID 22258010HCID 22258010, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6590Isobutyric Acid용매

실험 절차

Sodium borohydride (3.0 g) was added in 6 portions over 3 hours to a stirred solution of ethyl 2-amino-5-(phenylmethyl)thiophene-3-carboxylate in 2-methylpropanoic acid under nitrogen. The mixture was stirred at room temperature for 20 hours and was then diluted with water, neutralized with sodium bicarbonate and extracted with ethyl acetate four times. The organic extracts were dried over anhydrous magnesium sulfate, filtered and evaporated under reduced pressure. The residue was purified by column chromatography, eluting with diethyl ether:isohexane (1:19) to give the subtitle compound (2.80 g).

후처리

  1. extractionextracted with ethyl acetate four times
  2. dry with materialThe organic extracts were dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. customevaporated under reduced pressure
  5. customThe residue was purified by column chromatography
  6. washeluting with diethyl ether:isohexane (1:19)

출처 및 근거

ORD 기록
ord-6f0e3dc80e464515bcfff6f6f329ac9c
출처 데이터셋
uspto-grants-2006_01
특허 번호
US06984644B2

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