3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole → 3-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

HRID 1020947ノート

反応式

HRID 1020947 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([N+:18]([O-])=O)[CH:16]=3)[N:11]([C:21]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)([C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1>CO.C1(C)C=CC=CC=1.[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[C:17]3[C:12](=[CH:13][CH:14]=[C:15]([NH2:18])[CH:16]=3)[N:11]([C:21]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)[C:28]3[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=3)[N:10]=2)[CH:6]=[CH:5][N:4]=1

参加物

4

反応物 1

HCID 673446273-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole

生成物 1

HCID 583720003-(2-methoxypyridin-4-yl)-1-trityl-1H-indazol-5-ylamine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 21867641Toluene methanol溶媒

実験手順

To the stirred suspension of 3-(2-Methoxy-pyridin-4-yl)-5-nitro-1-trityl-1H-indazole 4BV (5.125 g, 10.0 mmole) in MeOH/toluene (50 mL/50 mL) was added 10% Pd/C (Degussa type, 0.5 g) at r.t. under dry N2 gas. The mixture was degassed and was stirred under a balloon inflated with H2 gas overnight. The catalyst was filtered through microfiber filter and was washed with MeOH and CH2Cl2. The filtrate was evaporated to dryness and a brown solid 5BV was obtained (5.0 g).

後処理

  1. customThe mixture was degassed
  2. custominflated with H2 gas overnight
  3. filtrationThe catalyst was filtered through microfiber
  4. filtrationfilter
  5. washwas washed with MeOH and CH2Cl2
  6. customThe filtrate was evaporated to dryness
  7. customa brown solid 5BV was obtained (5.0 g)

出典と根拠

ORDレコード
ord-311c9f53991841e99af52dc0f4531318
出典データセット
uspto-grants-2014_05
特許番号
US08716483B2

反応ノート

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