Methanol → RS-51324

HRID 27840노트

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HRID 27840 반응식
[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]

참가 물질

7

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 24386Thionyl ChlorideHCID 178502520HCID 178502520, 화합물

생성물 1

HCID 173875RS-51324

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

To 1 gram of 1-(2',6'-dichlorophenyl)-2-(2',3'-bismethoxycarbonylguanidino) 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.).

후처리

  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

출처 및 근거

ORD 기록
ord-fe32208c60404b3d8bafaaa59d7f9daa
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04224224

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