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Acetone → N-(2-t-Butyl-5-carbamoylphenyl)-3-[4-(1-hydroxybutyl)-2-methoxyphenyl]octanamide

HRID 1418153
ノート
印刷プレビュー

反応式

HRID 1418153 の反応式
[BH4-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[NH2:14])=[CH:9][C:8]=1[NH:16][C:17](=[O:38])[CH2:18][CH:19]([C:25]1[CH:30]=[CH:29][C:28]([C:31](=[O:35])[CH2:32][CH2:33][CH3:34])=[CH:27][C:26]=1[O:36][CH3:37])[CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])([CH3:6])([CH3:5])[CH3:4].CC(C)=O.C(OCC)(=O)C>C(O)C.CO>[C:3]([C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[NH2:14])=[CH:9][C:8]=1[NH:16][C:17](=[O:38])[CH2:18][CH:19]([C:25]1[CH:30]=[CH:29][C:28]([CH:31]([OH:35])[CH2:32][CH2:33][CH3:34])=[CH:27][C:26]=1[O:36][CH3:37])[CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])([CH3:5])([CH3:6])[CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 180AcetoneHCID 8857Ethyl AcetateHCID 4311764Sodium borohydrideHCID 19348622N-(2-t-Butyl-5-carbamoylphenyl)-3-[4-(1-oxobutyl)-2-methoxyphenyl]octanamide

生成物 1

HCID 19348575N-(2-t-Butyl-5-carbamoylphenyl)-3-[4-(1-hydroxybutyl)-2-methoxyphenyl]octanamide収率 98%

試薬・触媒・溶媒 2

HCID 702
Ethanol
溶媒
HCID 887Methanol溶媒

実験手順

70 mg (1.85 mmol) of sodium borohydride were added to a solution of 207 mg (0.418 mmol) of N-(2-t-butyl-5-carbamoylphenyl)-3-[4-(1-oxobutyl)-2-methoxyphenyl]octanamide (prepared as described in Example 99) in 5 ml of ethanol, and the resulting mixture was stirred for 3.5 hours. At the end of this time, the mixture was ice-cooled, acetone was added to the reaction mixture to decompose any excess of the reagent, and the solvent was removed by distillation under reduced pressure. The resulting residue was mixed with water and then extracted with ethyl acetate. The extract was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent was then removed by evaporation under reduced pressure. The residue thus obtained was purified by column chromatography through 15 g of silica gel using a gradient elution method, with mixtures of ethyl acetate and methanol ranging from 20:0 to 20:1 by volume as the eluent, to give 203 mg (yield 98%) of the title compound as crystals, melting at 153°-155° C.

後処理

  1. temperaturecooled
  2. customthe solvent was removed by distillation under reduced pressure
  3. additionThe resulting residue was mixed with water
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with a saturated aqueous solution of sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was then removed by evaporation under reduced pressure
  8. customThe residue thus obtained
  9. customwas purified by column chromatography through 15 g of silica gel using
  10. washa gradient elution method

出典と根拠

ORDレコード
ord-bcec41b6af4d47e39df01d1423022a6f
出典データセット
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05880147

反応ノート

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