Benzylamine → HCID 23347165、化合物

HRID 1855959

反応式

HRID 1855959 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][C:11]=1[O:12][CH2:13][CH2:14]Br)[CH2:7][OH:8])[CH3:2].[CH2:16]([NH2:23])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.C(OCC)(=O)C>CC(C)=O>[CH2:16]([NH:23][CH2:14][CH2:13][O:12][C:11]1[CH:10]=[CH:9][C:6]([CH2:7][OH:8])=[CH:5][C:4]=1[O:3][CH2:1][CH3:2])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

5

反応物 3

HCID 7504BenzylamineHCID 8857Ethyl AcetateHCID 543733553-Ethoxy-4-(2-bromoethoxy)benzyl alcohol

生成物 1

HCID 23347165HCID 23347165、化合物収率 74.7%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 27.5 g of 3-ethoxy-4-(2-bromoethoxy)benzyl alcohol and 53.5 g of benzylamine was heated to 130°-135° C. for 1.5 hours with stirring. After cooling the reaction mixture, 300 ml of ethyl acetate was added therein and the mixture was washed twice each time with 50 ml of water, dried with anhydrous sodium sulfate and distilled under reduced pressure to provide an orange oily product. To the product was added 50 ml of acetone to form crystals, which were recovered by filtration under suction to provide 22.5 g of N-benzyl-2-(2-ethoxy-4-hydroxymethylphenoxy)ethylamine having a melting point of 164°-167° C.

後処理

  1. temperaturewas heated to 130°-135° C. for 1.5 hours
  2. additionwas added
  3. washthe mixture was washed twice each time with 50 ml of water
  4. dry with materialdried with anhydrous sodium sulfate
  5. distillationdistilled under reduced pressure
  6. customto provide an orange oily product
  7. customto form crystals, which
  8. filtrationwere recovered by filtration under suction

出典と根拠

ORDレコード
ord-5c7d3d64f88c419b8bca76ac44892cca
出典データセット
uspto-grants-1980_08
特許番号
US04217305

関連ノート

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