1-Ethynylcyclohexylamine → HCID 12939913、化合物

HRID 67120

反応式

HRID 67120 の反応式
[C:1]([C:3]1[CH:13]=[C:12]([NH:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH:11]=[CH:10][C:4]=1[O:5][CH2:6][CH:7]1[O:9][CH2:8]1)#[N:2].[C:20]([C:22]1([NH2:28])[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1)#[CH:21]>C(O)C>[C:1]([C:3]1[CH:13]=[C:12]([NH:14][C:15](=[O:19])[CH:16]([CH3:18])[CH3:17])[CH:11]=[CH:10][C:4]=1[O:5][CH2:6][CH:7]([OH:9])[CH2:8][NH:28][C:22]1([C:20]#[CH:21])[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1)#[N:2]

参加物

4

反応物 2

HCID 1216911-EthynylcyclohexylamineHCID 233181271-[2-Cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane

生成物 1

HCID 12939913HCID 12939913、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

7.8 gm (0.03 mol) of 1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane were dissolved in 80 ml of ethanol, and after addition of 7.5 gm (0.06 mol) of 1-ethinyl-cyclohexyl-amine the mixture was refluxed for one hour. The solvent was then distilled off, and the residue was acidified with dilute HCl. After extraction with ethyl acetate the aqueous phase was made alkaline by addition of NaOH, whereby basic components precipitated in oily form. They were taken up in ethyl acetate, the organic phase was washed with water, dried over MgSO4, evaporated and the solid residue was recrystallized twice from acetonitrile.

後処理

  1. temperaturewas refluxed for one hour
  2. distillationThe solvent was then distilled off
  3. extractionAfter extraction with ethyl acetate the aqueous phase
  4. additionby addition of NaOH, whereby basic components
  5. customprecipitated in oily form
  6. washthe organic phase was washed with water
  7. dry with materialdried over MgSO4
  8. customevaporated
  9. customthe solid residue was recrystallized twice from acetonitrile

出典と根拠

ORDレコード
ord-1bc5ffdd6ad2418a94a352058c4ea0a0
出典データセット
uspto-grants-1982_08
特許番号
US04344964

関連ノート

読み込み中…