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cyclohexyl N-phenylcarbamate → Cyclohexyl N-cyclohexylcarbamate

HRID 1834153
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HRID 1834153 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>[Rh].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

4

반응물 1

HCID 246597cyclohexyl N-phenylcarbamate

생성물 1

HCID 3307288Cyclohexyl N-cyclohexylcarbamate수율 97%

시약·촉매·용매 2

HCID 23948Rhodium촉매HCID 3776Isopropanol용매

실험 절차

A mixture of 21.9 g. (0.10 mole) of cyclohexyl carbanilate, 100 ml. of 2-propanol, and 2.4 g. of 5% Rh on carbon was added to a 300-ml. Magne Drive autoclave. The vessel was sealed, purged first with nitrogen and then with hydrogen, and pressured with hydrogen to 700 psig. The autoclave was agitated at 25° and 500-800 psig for 0.4 hr., followed by an additional 0.9 hr. with little or no gas absorption. The autoclave was cooled and depressurized. The reaction product was removed and filtered through Celite filter aid to remove the catalyst. The solvent was removed in a rotary evaporator under vacuum. The white solid residue consisted of 21.9 g. (97% yield) of cyclohexyl cyclohexylcarbamate, m.p. 77°-78°.

후처리

  1. additionA mixture of 21.9 g
  2. customThe vessel was sealed
  3. custompurged first with nitrogen
  4. wait, followed by an additional 0.9 hr
  5. customwith little or no gas absorption
  6. temperatureThe autoclave was cooled
  7. customThe reaction product was removed
  8. filtrationfiltered through Celite
  9. filtrationfilter aid
  10. customto remove the catalyst
  11. customThe solvent was removed in a rotary evaporator under vacuum

출처 및 근거

ORD 기록
ord-b32730e07b7b4250b0bdb94f0839a41d
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04069240

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