Methanol → RS-51324

HRID 426979ノート

反応式

HRID 426979 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[CH:9](O)[CH2:10][NH:11][C:12]([NH:18]C(OC)=O)=[N:13][C:14]([O:16][CH3:17])=[O:15].S(Cl)(Cl)=O.CO.[OH-].[Na+]>C(Cl)Cl.O>[CH3:17][O:16][C:14]([NH:13][C:12]1[NH:18][CH:9]([C:3]2[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=2[Cl:8])[CH2:10][N:11]=1)=[O:15]

参加物

7

反応物 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 178502520HCID 178502520、化合物

生成物 1

HCID 173875RS-51324

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To 1 gram of 1-(2',6'-dichlorophenyl)-2-(2',3'-bis-methoxycarbonylguanidino) ethanol dissolved in 20 ml of methylene chloride was added dropwise with cooling at 0° C. 0.35 g of thionyl chloride. At the conclusion of the addition period, the solution was stirred for an additional 60 minutes at room temperature. After the addition of 20 ml of methyl alcohol, a solution of 0.5 g of sodium hydroxide in 2 ml of water was added and the resulting mixture refluxed for 60 minutes. The reaction solution was evaporated to low volume under vacuum and 50 ml of water added. The precipitated solid was collected, washed with methanol, followed by water and dried. 4,5-Dihydro-2-methoxycarbonylamino-5-(2',6'-dichlorophenyl)imidazole was isolated, 0.3 g, m.p. 229-230 (dec.).

後処理

  1. additionwas added dropwise
  2. additionAt the conclusion of the addition period
  3. temperaturethe resulting mixture refluxed for 60 minutes
  4. customThe reaction solution was evaporated to low volume under vacuum and 50 ml of water
  5. additionadded
  6. customThe precipitated solid was collected
  7. washwashed with methanol
  8. customdried

出典と根拠

ORDレコード
ord-c34448bbc8944692bb29a113d469c3ea
出典データセット
uspto-grants-1979_10
特許番号
US04172204

反応ノート

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