2-Bromoethanol → HCID 58277361, 화합물

HRID 1949224노트

반응식

HRID 1949224 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([OH:19])[CH:14]=3)=[CH:11][C:10]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:32][CH2:33][OH:34]>CC(C)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH2:32][CH2:33][OH:34])[CH:14]=3)=[CH:11][C:10]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 58277403HCID 58277403, 화합물

생성물 1

HCID 58277361HCID 58277361, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

100 mg (0.29 mmol) of the compound of Example 44A are provided in 2 ml of dry acetone, 44.4 mg (0.32 mmol) of potassium carbonate and 36.5 mg (0.29 mmol) of 2-bromoethanol are added, and the mixture is heated under reflux overnight. The reaction mixture is subsequently purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with the addition of 0.1% formic acid) and 13.1 mg of the title compound are obtained.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux overnight
  3. customThe reaction mixture is subsequently purified by preparative HPLC (RP18 column
  4. additionmobile phase: acetonitrile/water gradient with the addition of 0.1% formic acid) and 13.1 mg of the title compound
  5. customare obtained

출처 및 근거

ORD 기록
ord-7d9d1705d8e445d78b7d7d9fc7e3b1bf
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08399682B2

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