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cyclohexyl N-phenylcarbamate → Cyclohexyl N-cyclohexylcarbamate

HRID 1834153
ノート
印刷プレビュー

反応式

HRID 1834153 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 246597cyclohexyl N-phenylcarbamate

生成物 1

HCID 3307288Cyclohexyl N-cyclohexylcarbamate収率 97%

試薬・触媒・溶媒 2

HCID 23948Rhodium触媒HCID 3776Isopropanol溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-b32730e07b7b4250b0bdb94f0839a41d
出典データセット
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04069240

反応ノート

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