Tetrahydrofuran → HCID 69655662、化合物

HRID 11566

反応式

HRID 11566 の反応式
[C:1]([O:5][C:6](=[O:25])[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[CH:18]=[N:19][C:20]([C:23]#[N:24])=[CH:21][CH:22]=1)=[O:16])([CH3:4])([CH3:3])[CH3:2].C1COCC1>[Pd].CO>[C:1]([O:5][C:6](=[O:25])[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[CH:18]=[N:19][C:20]([CH2:23][NH2:24])=[CH:21][CH:22]=1)=[O:16])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 2

HCID 8028TetrahydrofuranHCID 69655660{2-[(6-Cyano-pyridine-3-carbonyl)-amino]-phenyl}-carbamic acid t-butyl ester

生成物 1

HCID 69655662HCID 69655662、化合物収率 87.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

In a flask, 2920 mg (8.72 mmol) {2-[(6-Cyano-pyridine-3-carbonyl)-amino]-phenyl}-carbamic acid t-butyl ester and 1000 mg Pd (10% on carbon) were placed under nitrogen and 10 ml THF and 120 ml methanol were added. The starting material was hydrogenated under atmospheric pressure and at rt for 3.5 h. The catalyst was filtered off. The solvent was evaporated and the residue was subjected to silica gel chromatography (toluene/isopropanol/NH3 (conc.) 16:20:1) to yield 2600 mg (7.6 mmol) {2-[(6-Aminomethyl-pyridine-3-carbonyl)-amino]-phenyl}-carbamic acid t-butyl ester; exact MW [M+H] calc'd: 343.18; MW found [M+H]: 343.2.

後処理

  1. filtrationThe catalyst was filtered off
  2. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-5d0d19c1f38d4ac39a2931cfcb53fdfb
出典データセット
uspto-grants-2006_08
特許番号
US07098247B2

関連ノート

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