Ethanol → HCID 69947292、化合物

HRID 1265285

反応式

HRID 1265285 の反応式
[C:1]([CH:9]([C:11](=O)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)C)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:19]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])(=[O:22])[NH:20][NH2:21].[CH3:28]CO>CC(O)=O.O>[C:24]([O:23][C:19](=[O:22])[NH:20][N:21]1[C:12]([C:17]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:28]=2)=[CH:11][CH:9]=[C:1]1[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)([CH3:27])([CH3:26])[CH3:25]

参加物

6

反応物 3

HCID 702EthanolHCID 70091tert-Butyl carbazateHCID 3446371,3-Diphenyl-2-methyl-1,3-propandione

生成物 1

HCID 69947292HCID 69947292、化合物収率 96%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 962Water溶媒

実験手順

A solution of dibenzoylethane (5 g, 21.0 mmol) and t-butyl carbazate (3.98 g, 30.1 mmol) in EtOH (170 mL) and AcOH (21 mL) was heated to reflux under Ar for 4.5 h, cooled to rt and diluted with water (400 mL). The resulting suspension was stirred under Ar at rt for 3 h, and then allowed to settle overnight at rt. The solid was filtered, washed with small portions of water and dried in vacuo to afford (2,5-Diphenyl-pyrrol-1-yl)-carbamic acid tert-butyl ester (6.72 g, 96%) as a white solid: 1H NMR (CDCl3, chemical shifts in ppm relative to TMS): 1.14 (s, 3H), 1.38 (s, 6H), 6.35 (s, 2H), 6.84 (bs, 2H), 7.29-7.53 (m, 10H).

後処理

  1. temperatureto reflux under Ar for 4.5 h
  2. waitto settle overnight at rt
  3. filtrationThe solid was filtered
  4. washwashed with small portions of water
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-0c2794cb66df4629b40f1a61c306bc4c
出典データセット
uspto-grants-2003_04
特許番号
US06545108B1

関連ノート

読み込み中…