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Water → HCID 15411702、化合物

HRID 1935721
ノート
印刷プレビュー

反応式

HRID 1935721 の反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([C:11](=[O:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]=2[N:4]=[C:3]1[CH2:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[BH4-].[Na+].O>CO>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]([OH:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]=2[N:4]=[C:3]1[CH2:19][CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 15411701HCID 15411701、化合物

生成物 1

HCID 15411702HCID 15411702、化合物収率 48.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a suspension of ethyl 3-(1-methyl-2-(2-phenylethyl)benzimidazol-4-yl)-3-oxopropanoate (0.80 g) obtained in Inventive Example 10 in anhydrous methanol (16 mL), was added sodium borohydride in small portions which was cooled in an ice bath. After stirring for 20 minutes at room temperature, the reaction solution was poured into water and concentrated under a reduced pressure. The thus obtained residue was extracted with ethyl acetate, and the organic layer was washed with water and brine in that order. The organic layer was dried over anhydrous sodium sulfate and then the solvent was evaporated under a reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain the title compound as white crystal (0.39 g).

後処理

  1. temperaturewas cooled in an ice bath
  2. concentrationconcentrated under a reduced pressure
  3. extractionThe thus obtained residue was extracted with ethyl acetate
  4. washthe organic layer was washed with water and brine in that order
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under a reduced pressure
  7. customThe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-efa1706a50fc440884434788071a507c
出典データセット
uspto-grants-2002_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06387938B1

反応ノート

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