反应 #607490

ord-3467facd1d4848b98500afe25c334c84

反应方程式

COC(=O)c1c(C(=O)OC)c2n(c1CCN1C(=O)c3ccccc3C1=O)CC(C)(C)C2
137k
COC(=O)c1c(C(=O)OC)c2n(c1CCN1C(=O)c3ccccc3C1=O)CC(C)(C)C2
dimethyl 5-(2-(1,3-dioxoisoindolin-2-yl)ethyl)-2,2-dimethyl-2,3-dihydro-1H-pyrrolizine-6,7-dicarboxylate
NN.O
hydrazine hydrate
COC(=O)c1c2c(n3c1CC(C)(C)C3)CCNC2=O
methyl 7,7-dimethyl-1-oxo-2,3,4,6,7,8-hexahydro-1H-pyrido[3,4-b]pyrrolizine-9-carboxylate

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling
  2. 2
    其他the reaction to RT
  3. 3
    过滤the resultant precipitate was filtered
  4. 4
    洗涤washed with ethanol
  5. 5
    浓缩The filtrate was concentrated

实验过程

To a solution of 137k (15.0 g, 35.4 mmol) in EtOH (100 mL) was added hydrazine hydrate (3.5 g, 70.8 mmol). See FIG. 2. The mixture was stirred at 90° C. for 2 h. After cooling the reaction to RT, the resultant precipitate was filtered and washed with ethanol. The filtrate was concentrated to give crude methyl 7,7-dimethyl-1-oxo-2,3,4,6,7,8-hexahydro-1H-pyrido[3,4-b]pyrrolizine-9-carboxylate 137l as a yellow solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09326985B2uspto-grants-2016_05