1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 178426239, 화합물

HRID 704783노트

반응식

HRID 704783 반응식
C(O[C@H:5]1[C@H:10]([N:11]2[CH2:15][CH2:14][NH:13][C:12]2=[N:16][C:17]#[N:18])[C:9]2[CH:19]=[C:20]([C:23]#[N:24])[CH:21]=[CH:22][C:8]=2[O:7][C:6]1([CH3:26])[CH3:25])(=O)C.N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1>[C:17]([N:16]=[C:12]1[NH:13][CH2:14][CH2:15][N:11]1[C:10]1[C:9]2[CH:19]=[C:20]([C:23]#[N:24])[CH:21]=[CH:22][C:8]=2[O:7][C:6]([CH3:26])([CH3:25])[CH:5]=1)#[N:18]

참가 물질

4

반응물 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 178476609HCID 178476609, 화합물

생성물 1

HCID 178426239HCID 178426239, 화합물수율 58.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a suspension of trans-3-acetoxy-4-(2-cyanoiminoimidazolidin-1-yl)-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.35 g) in toluene (7 ml) was added 1,8-diazabicyclo[5.4.0]undec-7-ene (0.19 ml) and the mixture was stirred under reflux for 2.5 hours. The solvent was evaporated in vacuo and the residue was dissolved in a mixture of ethyl acetate and water. The organic layer was separated, washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue was recrystallized from ethanol to give 4-(2-cyanoiminoimidazolidin-1-yl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile (0.17 g).

후처리

  1. temperatureunder reflux for 2.5 hours
  2. customThe solvent was evaporated in vacuo
  3. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
  4. customThe organic layer was separated
  5. washwashed with brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated in vacuo
  8. customThe residue was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-fb412fa564d84d598d9dcddd2b741430
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04988723

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