Water → HCID 57597232、化合物

HRID 1926065ノート

反応式

HRID 1926065 の反応式
[Cl:1][C:2]1[CH:17]=[C:16]([NH:18][C:19]2[C:20]3[N:27]([CH2:28][CH2:29][O:30][CH2:31][CH2:32][OH:33])[CH:26]=[CH:25][C:21]=3[N:22]=[CH:23][N:24]=2)[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([C:11](=[O:13])[CH3:12])[CH:8]=[CH:9][CH:10]=1.[BH4-].[Na+].O>CO>[Cl:1][C:2]1[CH:17]=[C:16]([NH:18][C:19]2[C:20]3[N:27]([CH2:28][CH2:29][O:30][CH2:31][CH2:32][OH:33])[CH:26]=[CH:25][C:21]=3[N:22]=[CH:23][N:24]=2)[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]([OH:13])[CH3:12])[CH:8]=[CH:9][CH:10]=1

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 57597191HCID 57597191、化合物

生成物 1

HCID 57597232HCID 57597232、化合物収率 96.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 1-{3-[2-chloro-4-({5-[2-(2-hydroxyethoxy)ethyl]-5H-pyrrolo[3,2-d]pyrimidin-4-yl}amino)phenoxy]phenyl}ethanone (233 mg) in methanol (5 mL) was added sodium borohydride (38 mg), and the mixture was stirred at room temperature for 2 hrs. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the obtained residue was crystallized from ethyl acetate-diethyl ether to give the title compound (225 mg) as a white powder.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe obtained residue was crystallized from ethyl acetate-diethyl ether

出典と根拠

ORDレコード
ord-ec51911483904750a5974d11a160f995
出典データセット
uspto-grants-2012_05
特許番号
US08178543B2

反応ノート

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