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2-Nitro-9h-fluoren-1-ol → 2-Amino-1-hydroxyfluorene

HRID 612682
笔记
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反应方程式

HRID 612682 反应方程式
[OH:1][C:2]1[C:14]2[CH2:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]=2[CH:5]=[CH:4][C:3]=1[N+:15]([O-])=O>CO.[Pd]>[NH2:15][C:3]1[CH:4]=[CH:5][C:6]2[C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[CH2:13][C:14]=2[C:2]=1[OH: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 2425562-Nitro-9h-fluoren-1-ol

产物 1

HCID 964522-Amino-1-hydroxyfluorene收率 81.2%

试剂、催化剂与溶剂 2

HCID 23938钯碳催化剂HCID 887Methanol溶剂

实验过程

To a solution of 1-hydroxy-2-nitrofluorene(250 mg, 1.23 mmol) in methanol(250 mL) was added 10% Pd/C (1 g). The mixture was flushed with argon, then hydrogen was bubbled through the solution for 10 min. and a hydrogen atmosphere was maintained at balloon pressure overnight. The mixture was filtered through celite and the celite was washed with methanol. The solvent was evaporated and chromatography of the resulting solid on silica gel (5%MeOH/CH2Cl2) gave the desired product(171 mg, 81.2%). 1H NMR (CD3OD): δ 7.60 (d, 1H), 7.47 (d, 1H), 7.28 (t, 1H), 7.18 (m, 2H), 6.82 (d, 1H), 3.76 (s, 2H).

本页导航参与物实验过程后处理来源与证据反应笔记

后处理

  1. customThe mixture was flushed with argon
  2. customhydrogen was bubbled through the solution for 10 min.
  3. temperaturea hydrogen atmosphere was maintained at balloon pressure overnight
  4. filtrationThe mixture was filtered through celite
  5. washthe celite was washed with methanol
  6. customThe solvent was evaporated

来源与证据

ORD记录
ord-efc5d5a0d5e74778b7532f7e49192a30
来源数据集
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
专利号
US06005008

反应笔记

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