HCID 13424017、化合物 → HCID 13490406、化合物

HRID 485368ノート

反応式

HRID 485368 の反応式
[CH3:1][C:2]1[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:8]2[N:4]([CH2:5][CH2:6][CH:7]2[C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH:3]=1.[CH2:20]1[C:27]2[N:23]([C:24]([C:28](Cl)=[O:29])=[CH:25][CH:26]=2)[CH2:22][CH2:21]1>C(Cl)Cl>[CH2:20]1[C:27]2[N:23]([C:24]([C:28]([C:3]3[N:4]4[C:8](=[C:9]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:2]=3[CH3:1])[CH:7]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:6][CH2:5]4)=[O:29])=[CH:25][CH:26]=2)[CH2:22][CH2:21]1

参加物

4

反応物 2

HCID 13424017HCID 13424017、化合物HCID 134904052,3-Dihydro-1H-pyrrolizine-5-carbonyl chloride

生成物 1

HCID 13490406HCID 13490406、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To an ice-bath cooled solution of diethyl 6-methyl-2,3-dihydro-1H-pyrrolizine-1,7-dicarboxylate (2.0 g, 0.0075 m) in methylene chloride (25 ml) was added stannic chloride (2.6 ml, 0.0225 m) all at once. A solution of 2,3-dihydro-1H-pyrrolizine-5-carbonyl chloride (1.1 g, 0.0075 m) in methylene chloride (10 ml) was then added dropwise, and the resultant mixture stirred cold for two hours, then at ambient temperatures overnight. The reaction mixture was then quenched with excess ice-H2O and ether, the organic layer removed, washed well with water, dried over sodium sulfate, filtered, and concentrated in vacuo to a residue. Trituration with either yielded 1.75 g of diethyl 5-(2,3-dihydro-1H-pyrrolizin-5-oyl)-6-methyl-2,3-dihydro-1H-pyrrolizine-1,7-dicarboxylate as a white solid.

後処理

  1. customat ambient temperatures overnight
  2. customThe reaction mixture was then quenched with excess ice-H2O and ether
  3. customthe organic layer removed
  4. washwashed well with water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo to a residue

出典と根拠

ORDレコード
ord-b71273306cbc4184829032b36600f215
出典データセット
uspto-grants-1985_08
特許番号
US04536512

反応ノート

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