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cyclohexyl N-phenylcarbamate → Cyclohexyl N-cyclohexylcarbamate

HRID 1834152
ノート
印刷プレビュー

反応式

HRID 1834152 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>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

3

反応物 1

HCID 246597cyclohexyl N-phenylcarbamate

生成物 1

HCID 3307288Cyclohexyl N-cyclohexylcarbamate収率 99%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-989b36abfb5441678a9181dd36cbece3
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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