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Sodium borohydride → HCID 66778107、化合物

HRID 2091389
ノート
印刷プレビュー

反応式

HRID 2091389 の反応式
[CH:1]1([C:4]2[CH:5]=[CH:6][C:7]3[O:11][C:10]([C:12](=[O:16])[CH:13]([CH3:15])[CH3:14])=[C:9]([CH3:17])[C:8]=3[CH:18]=2)[CH2:3][CH2:2]1.[BH4-].[Na+]>O1CCCC1.CO>[CH:1]1([C:4]2[CH:5]=[CH:6][C:7]3[O:11][C:10]([CH:12]([OH:16])[CH:13]([CH3:14])[CH3:15])=[C:9]([CH3:17])[C:8]=3[CH:18]=2)[CH2:2][CH2:3]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 2

HCID 4311764Sodium borohydrideHCID 66777760HCID 66777760、化合物2 回

生成物 1

HCID 66778107HCID 66778107、化合物収率 50%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

1-(5-Cyclopropyl-3-methyl-1-benzofuran-2-yl)-2-methylpropan-1-one (0.80 g) synthesized in the above-mentioned (1) was dissolved in tetrahydrofuran (10 mL) and methanol (1 mL), and sodium borohydride (90%, 0.34 g) was added to the solution under ice-cooling. The ice bath was removed, and the reaction mixture was stirred at room temperature for 1 hr then ice-cooled again, and water (1 mL) and 1N hydrochloric acid (5 mL) were carefully added to the mixture, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure to give the title object compound (0.4 g, 50%) as a yellow oil.

後処理

  1. temperaturecooling
  2. customThe ice bath was removed
  3. temperatureice-cooled again
  4. additionwater (1 mL) and 1N hydrochloric acid (5 mL) were carefully added to the mixture
  5. extractionthe mixture was extracted with ethyl acetate
  6. washThe extract was washed with saturated brine
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-8dac8f3adcd84a27a838827c80783529
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436043B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート