1-Ethynylcyclohexylamine → HCID 12939913, 화합물

HRID 67120노트

반응식

HRID 67120 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 12939913HCID 12939913, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1bc5ffdd6ad2418a94a352058c4ea0a0
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344964

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