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

HRID 1385398
ノート
印刷プレビュー

反応式

HRID 1385398 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 2425562-Nitro-9h-fluoren-1-ol

生成物 1

HCID 964522-Amino-1-hydroxyfluorene収率 81.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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): d 7.60 (d, 1H), 7.47 (d, 1H), 7.28 (t, 1H), 7.18 (m, 2H), 6.82 (d, 1H), 3.76 (s, 2H).

後処理

  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

出典と根拠

ORDレコード
ord-cdb6d75d3e61431fa651e4357e13d8dc
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06262113B1

反応ノート

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