HCID 13424017, 화합물 → HCID 13490406, 화합물

HRID 485368노트

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HRID 485368 반응식
[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

참가 물질

4

반응물 2

HCID 13424017HCID 13424017, 화합물HCID 134904052,3-Dihydro-1H-pyrrolizine-5-carbonyl chloride

생성물 1

HCID 13490406HCID 13490406, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b71273306cbc4184829032b36600f215
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04536512

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