1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 178426239、化合物

HRID 704783ノート

反応式

HRID 704783 の反応式
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]

参加物

4

反応物 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 178476609HCID 178476609、化合物

生成物 1

HCID 178426239HCID 178426239、化合物収率 58.5%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-fb412fa564d84d598d9dcddd2b741430
出典データセット
uspto-grants-1991_01
特許番号
US04988723

反応ノート

読み込み中…