2-Bromoethanol → HCID 58277361、化合物

HRID 1949224ノート

反応式

HRID 1949224 の反応式
[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

参加物

5

反応物 3

HCID 108982-BromoethanolHCID 11430Potassium CarbonateHCID 58277403HCID 58277403、化合物

生成物 1

HCID 58277361HCID 58277361、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-7d9d1705d8e445d78b7d7d9fc7e3b1bf
出典データセット
uspto-grants-2013_03
特許番号
US08399682B2

反応ノート

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