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

HRID 1613184
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HRID 1613184 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7037BenzhydrolHCID 118072-Amino-2-methyl-1-propanolHCID 521998p-Toluenesulfonic acid monohydrate

생성물 1

HCID 197753022-Amino-1-diphenylmethoxy-2-methylpropane수율 69.3%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-62721b2bbdd94ffda5d2117873e8a9c7
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05192765

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