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Methylamine → 1-Methylamino-3-phenoxy-propan-2-ol

HRID 2286354
ノート
印刷プレビュー

反応式

HRID 2286354 の反応式
[O:1]1[CH:3]([CH2:4][O:5][C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH2:2]1.[CH3:12][NH2:13]>C(O)C.O>[CH3:12][NH:13][CH2:2][CH:3]([OH:1])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=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 6329MethylamineHCID 31217Phenyl glycidyl ether

生成物 1

HCID 31483571-Methylamino-3-phenoxy-propan-2-ol

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

To a solution of 1,2-epoxy-3-phenoxypropane (15 g), in ethanol (50 ml) was added 25-30% methylamine in water (50 ml) and the mixture heated under reflux for 1 h. The ethanol was removed in vacuo and the residue acidified with 2 N hydrochloric acid. The aqueous solution was extracted with ether acetate then made alkaline with 2 N sodium hydroxide and extracted into ether. The combined ethereal extracts were dried (Na2SO4), filtered and evaporated to give a semi-solid (14.8 g). The product was distilled in vacuo to give the title compound as white crystals b.p. 110°/0.07 mm, m.p. 74°-77° (9 g).

後処理

  1. temperaturethe mixture heated
  2. temperatureunder reflux for 1 h
  3. customThe ethanol was removed in vacuo
  4. extractionThe aqueous solution was extracted with ether acetate
  5. extractionextracted into ether
  6. dry with materialThe combined ethereal extracts were dried (Na2SO4)
  7. filtrationfiltered
  8. customevaporated

出典と根拠

ORDレコード
ord-4a7a4b5041404e9c9e9883b0b4b46057
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04265891

反応ノート

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