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

HRID 1166778
ノート
印刷プレビュー

反応式

HRID 1166778 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

(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.

後処理

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

出典と根拠

ORDレコード
ord-ef37ae2076bf4b858a4c5b2d5dfaca70
出典データセット
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06613942B1

反応ノート

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