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benzyl spiro[1H-chromeno[4,3-c]pyrazole-4,4'-piperidine]-1'-carboxylate → 1H-spiro[chromeno[4,3-c]pyrazole-4,4'-piperidine]

HRID 1908016
笔记
打印预览

反应方程式

HRID 1908016 反应方程式
[N:1]1(C(OCC2C=CC=CC=2)=O)[CH2:6][CH2:5][C:4]2([C:18]3[CH:17]=[N:16][NH:15][C:14]=3[C:13]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[O:7]2)[CH2:3][CH2:2]1>CO.[Pd]>[NH:1]1[CH2:6][CH2:5][C:4]2([C:18]3[CH:17]=[N:16][NH:15][C:14]=3[C:13]3[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=3[O:7]2)[CH2:3][CH2:2]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 58550771benzyl spiro[1H-chromeno[4,3-c]pyrazole-4,4'-piperidine]-1'-carboxylate

产物 1

HCID 585517941H-spiro[chromeno[4,3-c]pyrazole-4,4'-piperidine]收率 80%

试剂、催化剂与溶剂 2

HCID 23938钯碳催化剂HCID 887Methanol溶剂

实验过程

A mixture of benzyl spiro[1H-chromeno[4,3-c]pyrazole-4,4′-piperidine]-1′-carboxylate (1.11 g, 2.96 mmol) and palladium (10% wt on carbon, 157 mg, 0.15 mmol) in MeOH (15 mL) was set under hydrogen (1 atm) and stirred vigorously at room temperature for 3 hours. The reaction mixture was filtered through Celite and the filtrate was concentrated to afford 1H-spiro[chromeno[4,3-c]pyrazole-4,4′-piperidine] (570 mg, 80%). ESI-MS m/z calc. 241.1. found 242.5 (M+1)+; Retention time: 0.42 minutes (3 min run).

后处理

  1. filtrationThe reaction mixture was filtered through Celite
  2. concentrationthe filtrate was concentrated

来源与证据

ORD记录
ord-bd66f55436854f29bcfb0b9d567872c4
来源数据集
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US08598164B2

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