Acetic Acid → 4-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

HRID 1492328

반응식

HRID 1492328 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 855407454-Cyclohexylcyclohexylidenephosphorohydrazidic Acid, Diethyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cf31f567f2c54bad8315e41ad9286a53
출처 데이터셋
uspto-grants-1994_12
특허 번호
US05373095

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