HCID 68183820、化合物 → HCID 68184017、化合物

HRID 879014ノート

反応式

HRID 879014 の反応式
[Cl:1][C:2]1[CH:23]=[CH:22][CH:21]=[C:20]([Cl:24])[C:3]=1[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([O:17]C)=[C:11]([C:14]([OH:16])=[O:15])[CH:12]=2)[C:7]([CH3:19])=[N:6]1.[Br-].[Br-].[Br-].B>C(Cl)Cl>[Cl:24][C:20]1[CH:21]=[CH:22][CH:23]=[C:2]([Cl:1])[C:3]=1[CH2:4][N:5]1[C:13]2[C:8](=[CH:9][C:10]([OH:17])=[C:11]([C:14]([OH:16])=[O:15])[CH:12]=2)[C:7]([CH3:19])=[N:6]1

参加物

4

反応物 2

HCID 68183820HCID 68183820、化合物HCID 178419136HCID 178419136、化合物

生成物 1

HCID 68184017HCID 68184017、化合物収率 52%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

To a suspension of the compound [179](7.4 mg) in methylenechloride (0.2 mL) was added 1M methylenechloride solution of borane tribromide (0.2 mL) under ice-cooling, and then the reaction mixture was stirred at 0° C. for 3 hours. The reaction mixture was quenched with water, and extracted with ethyl acetate. The obtained organic layer was dried over anhydrous sodium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The obtained residue was purified by reverse phase preparative liquid chromatography to give the titled compound (3.7 mg) as a pale brown solid.

後処理

  1. temperaturecooling
  2. customThe reaction mixture was quenched with water
  3. extractionextracted with ethyl acetate
  4. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThe obtained residue was purified by reverse phase preparative liquid chromatography

出典と根拠

ORDレコード
ord-6bf9455997394067a6ef658c6334f17a
出典データセット
uspto-grants-2015_03
特許番号
US08987473B2

反応ノート

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