Water → 2-(4-Hydroxyphenoxy)-3-methylquinoxaline

HRID 64582

반응식

HRID 64582 반응식
C([O:8][C:9]1[CH:26]=[CH:25][C:12]([O:13][C:14]2[C:23]([CH3:24])=[N:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)=[CH:11][CH:10]=1)C1C=CC=CC=1.O>C(Cl)Cl>[OH:8][C:9]1[CH:10]=[CH:11][C:12]([O:13][C:14]2[C:23]([CH3:24])=[N:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)=[CH:25][CH:26]=1

참가 물질

4

반응물 2

HCID 962WaterHCID 136705372-(4-Benzyloxyphenoxy)-3-methylquinoxaline

생성물 1

HCID 136705382-(4-Hydroxyphenoxy)-3-methylquinoxaline수율 50.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A solution of 12.5 g (0.05 mole) borontribromide in 100 cc methylene chloride was added, over a period of 40 minutes, to a well stirred, cold (-62° C.) solution of 17.1 g 2-(4-benzyloxyphenoxy)-3-methylquinoxaline (0.05 mole) in 400 cc methylene chloride. When the addition was complete, the temperature of the reaction was allowed to rise slowly (2 hours) to room temperature. The reaction mixture was then poured into 1 liter of water and an additional 500 cc of methylene chloride was added. The mixture was stirred vigorously for 40 minutes and the insoluble solid was filtered. Crystallization from an ethanol-water mixture (1:1) gave 6.4 g of product, m.p. 175°-178° C.

후처리

  1. additionWhen the addition
  2. custom(2 hours)
  3. customto room temperature
  4. stirringThe mixture was stirred vigorously for 40 minutes
  5. filtrationthe insoluble solid was filtered
  6. customCrystallization from an ethanol-water mixture (1:1)

출처 및 근거

ORD 기록
ord-2e50a64fef51404880287fa09ec46d4f
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609396

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