Urea → HCID 19101100、化合物

HRID 1588058ノート

反応式

HRID 1588058 の反応式
[CH3:1][C:2]([CH3:14])([C:4](=[O:13])[CH:5](Br)[C:6](=O)[C:7]([CH3:10])([CH3:9])[CH3:8])[CH3:3].[NH2:15][C:16]([NH2:18])=[O:17]>CN(C=O)C>[NH2:18][C:16]1[O:17][C:5]([C:4](=[O:13])[C:2]([CH3:14])([CH3:3])[CH3:1])=[C:6]([C:7]([CH3:10])([CH3:9])[CH3:8])[N:15]=1

参加物

4

反応物 2

HCID 1176UreaHCID 546382Bromo-dipivaloylmethane

生成物 1

HCID 19101100HCID 19101100、化合物収率 42.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2,2,6,6-tetramethyl-4-bromo-3,5-heptanedione (70 g) and urea (77 g) in DMF (500 mL) is heated at 110°-120° C. overnight. The reaction mixture is cooled and poured into ice water (1500 mL) and the resulting precipitate is collected by filtration and air dried. The solid is rinsed with hexane (1000 mL) and then with isopropyl ether (200 mL) and dried under vacuum overnight to give 1-[2-amino-4-(1,1-dimethylethyl)-5-oxazolyl]-2,2 dimethyl-1-propanone (25.5 g, 42%); mp 248°-250° C.

後処理

  1. temperatureis heated at 110°-120° C. overnight
  2. temperatureThe reaction mixture is cooled
  3. filtrationthe resulting precipitate is collected by filtration and air
  4. customdried
  5. washThe solid is rinsed with hexane (1000 mL)
  6. dry with materialwith isopropyl ether (200 mL) and dried under vacuum overnight

出典と根拠

ORDレコード
ord-8c0f876f1b9349c4af480af252b1ced3
出典データセット
uspto-grants-1993_06
特許番号
US05220025

反応ノート

読み込み中…