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Bromoacetyl chloride → (3R)-N-(1-benzylpyrrolidin-3-yl)-2-bromoacetamide hydrochloride

HRID 1166778
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HRID 1166778 반응식
[CH2:1]([N:8]1[CH2:12][CH2:11][C@@H:10]([NH2:13])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:14][CH2:15][C:16]([Cl:18])=[O:17]>ClCCl>[ClH:18].[CH2:1]([N:8]1[CH2:12][CH2:11][C@@H:10]([NH:13][C:16](=[O:17])[CH2:15][Br:14])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 89602Bromoacetyl chlorideHCID 1519354(3R)-1-benzylpyrrolidin-3-amine

생성물 1

HCID 67483732(3R)-N-(1-benzylpyrrolidin-3-yl)-2-bromoacetamide hydrochloride수율 72.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

(R)-(−)-1-Benzyl-3-aminopyrrolidine (5 g, 28 mmol) was dissolved in dichloromethane (10 ml). To this solution, a solution of bromoacetyl chloride (4.55 g, 28 mmol) in dichloromethane (5 ml) was added at room temperature. The mixture was stirred at room temperature for 16 hours. The mixture was filtered, washed with dichloromethane and dried in vacuo to afford 6.8 g (72%) of (3R)-N-(1-benzylpyrrolidin-3-yl)-2-bromoacetamide hydrochloride as a solid which was used directly in the next step. 4-Hydroxy-2-methoxybenzaldehyde (2.05 g , 13 mmol) was dissolved in DMF (7 ml) and potassium carbonate (6.2 g, 45 mmol) was added followed by a suspension of the above (3R)-N-(1-Benzylpyrrolidin-3-yl)-2-bromoacetamide hydrochloride (3.0 g, 9 mmol) in DMF (16 ml). The resulting mixture was stirred at room temperature for 16 hours. The mixture was then partitioned between water (100 ml) and ethyl acetate (30 ml). The aqueous phase was extracted with ethyl acetate (2×20 ml) and the combined organic extracts were washed with saturated sodium chloride (3×15 ml), dried (MgSO4) and concentrated in vacuo. The residue was crystallized from diethyl ether to afford 2.11 g (64%) (R)-N-(1-benzylpyrrolidin-3-yl)-2-(4-formyl-3-methoxyphenoxy)acetamide as a solid. M.p.: 98-101° C.

후처리

  1. filtrationThe mixture was filtered
  2. washwashed with dichloromethane
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-ef37ae2076bf4b858a4c5b2d5dfaca70
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06613942B1

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