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Benzhydrol → 2-Amino-1-diphenylmethoxy-2-methylpropane

HRID 1613184
ノート
印刷プレビュー

反応式

HRID 1613184 の反応式
[NH2:1][C:2]([CH3:6])([CH3:5])[CH2:3][OH:4].[CH:7](O)([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[NH2:1][C:2]([CH3:6])([CH3:5])[CH2:3][O:4][CH:7]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=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 7037BenzhydrolHCID 118072-Amino-2-methyl-1-propanolHCID 521998p-Toluenesulfonic acid monohydrate

生成物 1

HCID 197753022-Amino-1-diphenylmethoxy-2-methylpropane収率 69.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A mixture of 2-amino-2-methylpropanol (89.1 g), benzhydrol (190 g) and para-toluenesulphonic acid monohydrate (200 g) in toluene (1200 ml) was heated under reflux in a Dean-Stark apparatus for four hours and evaporated. The residue was partitioned between ether and water and the organic layer was washed with water and extracted into 10% aqueous citric acid. The acidic extract was washed with ether, basified with solid sodium carbonate and extracted into ether. The organic extract was washed with water, dried over sodium sulphate and evaporated to give the title compound as a pale yellow oil (177 g, 69%) which was characterised by its 1H-n.m.r. spectrum.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux in a Dean-Stark apparatus for four hours
  3. customevaporated
  4. customThe residue was partitioned between ether and water
  5. washthe organic layer was washed with water
  6. extractionextracted into 10% aqueous citric acid
  7. extractionThe acidic extract
  8. washwas washed with ether
  9. extractionextracted into ether
  10. extractionThe organic extract
  11. washwas washed with water
  12. dry with materialdried over sodium sulphate
  13. customevaporated

出典と根拠

ORDレコード
ord-62721b2bbdd94ffda5d2117873e8a9c7
出典データセット
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05192765

反応ノート

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