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cyclohexyl N-phenylcarbamate → Cyclohexyl N-cyclohexylcarbamate

HRID 1834152
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반응식

HRID 1834152 반응식
[C:1](=[O:16])([O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]1)[NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>CC(O)C>[CH:3]1([NH:2][C:1](=[O:16])[O:9][CH:10]2[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 246597cyclohexyl N-phenylcarbamate

생성물 1

HCID 3307288Cyclohexyl N-cyclohexylcarbamate수율 99%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 21.9 g. (0.10 mole) of cyclohexyl carbanilate, 77 ml. of 2-propanol, and 3.0 g. of 5% on carbon was added to a 0.5-1., glass, low pressure, Parr (trademark) shaker bottle. The apparatus was assembled, purged first with nitrogen and then with hydrogen, and pressured with hydrogen to 50 psig. The reaction mixture was agitated at room temperature and 50 to 25 psig for 3.0 hr., followed by an additional 0.8 hr. with little or no gas absorption. The reaction product was filtered through Celite filter aid to remove the catalyst. The solvent was removed in a rotary evaporator under vacuum. The solid residue consisted of 22.3 g. (99% yield) of cyclohexyl cyclohexylcarbamate, m.p. 77°-78°. Anal. Calcd. for C13H23NO2 : C, 69.29; H, 10.30; N, 6.21. Found: C, 69.43; H, 10.10; N, 6.20.

후처리

  1. additionA mixture of 21.9 g
  2. additionof 5% on carbon was added to a 0.5-1
  3. custompurged first with nitrogen
  4. wait, followed by an additional 0.8 hr
  5. customwith little or no gas absorption
  6. filtrationThe reaction product was filtered through Celite
  7. filtrationfilter aid
  8. customto remove the catalyst
  9. customThe solvent was removed in a rotary evaporator under vacuum

출처 및 근거

ORD 기록
ord-989b36abfb5441678a9181dd36cbece3
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04069240

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