Cyclopropylamine → HCID 45087015、化合物

HRID 859876ノート

反応式

HRID 859876 の反応式
[CH2:1]([N:8]1[CH2:12][C@H:11]([CH3:13])[C@@H:10]([C:14]([OH:16])=O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:17]1([NH2:20])[CH2:19][CH2:18]1.C(N=C=NCCCN(C)C)C.Cl>ClCCl>[CH2:1]([N:8]1[CH2:12][C@H:11]([CH3:13])[C@@H:10]([C:14]([NH:20][CH:17]2[CH2:19][CH2:18]2)=[O:16])[CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 69828CyclopropylamineHCID 1515523trans-1-Benzyl-4-methyl-pyrrolidine-3-carboxylic acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride

生成物 1

HCID 45087015HCID 45087015、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(3R,4R)-1-Benzyl-4-methyl-3-pyrrolidinecarboxylic acid (6.27 g) was suspended in dichloromethane (250 mL). To this suspension, cyclopropylamine (1.76 mL) and hydrochloric acid 1-ethyl-(3-dimethylaminopropyl)carbodiimide (12.2 g) were sequentially added and the mixture was stirred at room temperature for 4 hours. Subsequently, the reaction mixture was washed with water, was dried over anhydrous sodium sulfate, and was then concentrated under reduced pressure. The resulting residue was purified on a silica gel column (ethyl acetate: methanol=10:1) to give 3.32 g of (3R,4R)-1-benzyl-N-cyclopropyl-4-methyl-3-pyrrolidinecarboxamide as a white crystal.

後処理

  1. washSubsequently, the reaction mixture was washed with water
  2. dry with materialwas dried over anhydrous sodium sulfate
  3. concentrationwas then concentrated under reduced pressure
  4. customThe resulting residue was purified on a silica gel column (ethyl acetate: methanol=10:1)

出典と根拠

ORDレコード
ord-7c2e2d0048fd4424b6c5c657a59f4b0c
出典データセット
uspto-grants-2006_12
特許番号
US07153851B2

反応ノート

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