Acetic Acid → 4-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

HRID 1614463

反応式

HRID 1614463 の反応式
[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(O)(=O)C.[P:18]([NH:26][NH2:27])(=[O:25])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21]>C(Cl)Cl>[CH:1]1([CH:7]2[CH2:12][CH2:11][C:10](=[N:27][NH:26][P:18](=[O:25])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21])[CH2:9][CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 41690(1,1'-Bicyclohexyl)-4-oneHCID 143340Phosphorohydrazidic acid, diethyl ester

生成物 1

HCID 855407454-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 4-cyclohexylcyclohexanone (27.04 g) and acetic acid (3 ml) in CH2Cl2 (400 ml) was added a solution of diethyl phosphorohydrazidate (28.91 g) in CH2Cl2 (100 ml). The reaction was stirred at room temperature for 27 hours and then was concentrated under reduced pressure. Toluene was added (2×) and removed under reduced pressure in order to aid in the removal of acetic acid by co-distillation. The residual yellow liquid was the product and was used without further purification. TLC Rf=0.52 (20% acetone in CH2Cl2, silica gel).

後処理

  1. concentrationwas concentrated under reduced pressure
  2. additionToluene was added (2×)
  3. customremoved under reduced pressure in order
  4. customto aid in the removal of acetic acid by co-distillation
  5. customwas used without further purification

出典と根拠

ORDレコード
ord-cdb1b8a10ee54fd08606c2a81d50cb77
出典データセット
uspto-grants-1993_03
特許番号
US05196542

関連ノート

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