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Sodium borohydride → 3,5-Dimethoxy-4-(methylamino)-alpha-[(methylsulfonyl)-methyl]-benzyl alcohol

HRID 542974
ノート
印刷プレビュー

反応式

HRID 542974 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:13](=[O:19])[CH2:14][S:15]([CH3:18])(=[O:17])=[O:16])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[NH:9][CH3:10].[BH4-].[Na+]>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[NH:9][CH3:10])[CH:13]([OH:19])[CH2:14][S:15]([CH3:18])(=[O:17])=[O:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 212809593',5'-Dimethoxy-4'-(methylamino)-2-(methylsulfonyl)-acetophenone

生成物 1

HCID 538586323,5-Dimethoxy-4-(methylamino)-alpha-[(methylsulfonyl)-methyl]-benzyl alcohol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A suspension of 31 g. of 3',5'-dimethoxy-4'-(methylamino)-2-(methylsulfonyl)-acetophenone and 16.3 g. of sodium borohydride in 600 ml. of ethanol was stirred at room temperature for 16 hours. The solution was diluted with 600 ml. of water and the alcohol was removed by distillation under vacuum. The crystals formed were filtered with suction, washed with water and dried, whereby there was obtained 3,5-dimethoxy-4-(methylamino)-α-[(methylsulfonyl)-methyl]-benzyl alcohol having a melting point of 141°-142° C.

後処理

  1. additionA suspension of 31 g
  2. additionThe solution was diluted with 600 ml
  3. customof water and the alcohol was removed by distillation under vacuum
  4. customThe crystals formed
  5. filtrationwere filtered with suction
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-e2bc2d8740504923bb08c1d57e8fe3db
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04659818

反応ノート

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