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HCID 21584328,化合物 → HCID 21584267,化合物

HRID 583258
笔记
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反应方程式

HRID 583258 反应方程式
[ClH:1].[N+:2]([C:5]1[CH:18]=[CH:17][C:8]2[CH2:9][CH:10]3[N:15]([CH2:16][C:7]=2[CH:6]=1)[CH2:14][CH2:13][CH2:12][CH2:11]3)([O-])=O>C(O)C.[Pd]>[ClH:1].[CH2:11]1[CH:10]2[N:15]([CH2:16][C:7]3[CH:6]=[C:5]([NH2:2])[CH:18]=[CH:17][C:8]=3[CH2:9]2)[CH2:14][CH2:13][CH2:12]1
参与物实验过程后处理来源与证据反应笔记

参与物

4

反应物 1

HCID 21584328HCID 21584328,化合物

产物 1

HCID 21584267HCID 21584267,化合物收率 95.3%

试剂、催化剂与溶剂 2

HCID 23938钯碳催化剂HCID 702乙醇溶剂

实验过程

8-Nitro-1,3,4,6,11,11a-hexahydro-2H-benzo[b]quinolizine hydrochloride (2.93 g, 10.9 mmol) was dissolved in ethanol (150 ml) and 10% palladium-on-carbon (0.4 g) was added and the solution was shaken on a Parr Hydrogenator for 2 h. The catalyst was filtered off and the catalyst was washed with water. The filtrate was concentrated and absolute ethanol was added and evaporated to drive off excess water. The resulting solid was taken up in hot ethanol (75 ml) and ether (100 ml) was added slowly. The precipitate which formed was collected and dried in the air to give the title compound as an off-white solid (2.48 g, 95%), m.p. 241-3° C. (dec.).

后处理

  1. filtrationThe catalyst was filtered off
  2. washthe catalyst was washed with water
  3. concentrationThe filtrate was concentrated
  4. additionabsolute ethanol was added
  5. customevaporated
  6. additionether (100 ml) was added slowly
  7. customThe precipitate which formed
  8. customwas collected
  9. customdried in the air

来源与证据

ORD记录
ord-31dbfbf0d2d845288c6f33f8219b38a0
来源数据集
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
专利号
US05929085

反应笔记

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本页导航参与物实验过程后处理来源与证据反应笔记