HCID 178458534、化合物 → HCID 178458533、化合物

HRID 1644595

反応式

HRID 1644595 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:26][CH:27]([CH3:29])[CH3:28])=[C:13]([C:15]2[NH:25][C:18]3=[N:19][CH:20]=[C:21]([CH2:23][OH:24])[CH:22]=[C:17]3[N:16]=2)[CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>ClCCl.O=[Mn]=O>[CH2:1]([O:8][C:9]1[CH:10]=[CH:11][C:12]([O:26][CH:27]([CH3:29])[CH3:28])=[C:13]([C:15]2[NH:25][C:18]3=[N:19][CH:20]=[C:21]([CH:23]=[O:24])[CH:22]=[C:17]3[N:16]=2)[CH:14]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 1

HCID 178458534HCID 178458534、化合物

生成物 1

HCID 178458533HCID 178458533、化合物収率 70.4%

試薬・触媒・溶媒 2

HCID 14801Manganese dioxide触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of {2-[5-(benzyloxy)-2-isopropoxyphenyl]-3H-imidazo[4,5-b]pyridin-6-yl}methanol (1.0 g) in dichloromethane (50 ml) was added manganese peroxide (2.3 g), and the mixture was stirred at room temperature for 8 hr. The insoluble material was removed by filtration, and the filtrate was concentrated. The obtained crude crystals were washed with diethyl ether to give the title compound (0.70 g, yield 69%) as colorless crystals. melting point 170-171° C. purity 87%. M+H: 388. 1H NMR (CDCl3) δ: 1.52 (6H, d, J=6.0 Hz), 4.76-4.85 (1H, m), 5.17 (2H, s), 7.03-7.07 (1H, m), 7.11-7.16 (1H, m), 7.31-7.52 (5H, m), 8.20 (1H, d, J=3.2 Hz), 8.53 (1H, s), 8.88 (1H, d, J=1.5 Hz), 10.19 (1H, s).

後処理

  1. customThe insoluble material was removed by filtration
  2. concentrationthe filtrate was concentrated
  3. customThe obtained crude crystals
  4. washwere washed with diethyl ether

出典と根拠

ORDレコード
ord-0eb5253243204447a038b19ebd1173d0
出典データセット
uspto-grants-2012_02
特許番号
US08124617B2

関連ノート

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