Water → 3-(1-Adamantyl)-4-methoxyaniline

HRID 1756447ノート

反応式

HRID 1756447 の反応式
[C:1]12([C:11]3[CH:12]=[C:13]([CH:21]=[CH:22][C:23]=3[O:24][CH3:25])[NH:14]C(=O)C(F)(F)F)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.O.[OH-].[K+]>CO>[C:1]12([C:11]3[CH:12]=[C:13]([CH:21]=[CH:22][C:23]=3[O:24][CH3:25])[NH2:14])[CH2:2][CH:3]3[CH2:4][CH:5]([CH2:6][CH:7]([CH2:9]3)[CH2:8]1)[CH2:10]2

参加物

5

反応物 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 190682803-(1-adamantyl)4-methoxy-N-(trifluoroacetyl)aniline

生成物 1

HCID 80271163-(1-Adamantyl)-4-methoxyaniline

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

11.03 g (31.2 mmol) of 3-(1-adamantyl)4-methoxy -N-(trifluoroacetyl)aniline dissolved in 40 ml of methanol and 160 ml of water are treated with 7.12 g (51.5 mmol) of potassium hydroxide. The reaction medium is heated to 50° C. for 20 hours and then 80° C. for 18 hours. After evaporation to dryness, the residue is taken up with ethyl ether, the insoluble matter is filtered off and the filtrate is dried over magnesiumsulphate and evaporated. The solid is washed in hexane to yield, after drying, 7.44 g (93%) of 3-(1-adamantyl)-4-methoxyaniline, melting point 140°-141° C.

後処理

  1. customAfter evaporation to dryness
  2. filtrationthe insoluble matter is filtered off
  3. dry with materialthe filtrate is dried over magnesiumsulphate
  4. customevaporated
  5. washThe solid is washed in hexane
  6. customto yield
  7. customafter drying

出典と根拠

ORDレコード
ord-2d80fc7d1b8149999c9678d4fdcc4f8b
出典データセット
uspto-grants-1995_08
特許番号
US05439925

反応ノート

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