Ethanol → HCID 69947292, 화합물

HRID 1265285

반응식

HRID 1265285 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 69947292HCID 69947292, 화합물수율 96%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0c2794cb66df4629b40f1a61c306bc4c
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06545108B1

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