4-Nitrophthalic acid anhydride → 1-Cyclohexyl-4-(4-nitrophthalimido)piperidine

HRID 972818ノート

反応式

HRID 972818 の反応式
[NH2:1][CH:2]1[CH2:7][CH2:6][N:5]([CH:8]2[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]2)[CH2:4][CH2:3]1.[N+:14]([C:17]1[CH:18]=[C:19]2[C:24](=O)[O:23][C:21](=[O:22])[C:20]2=[CH:26][CH:27]=1)([O-:16])=[O:15]>C(Cl)(Cl)Cl>[CH:8]1([N:5]2[CH2:6][CH2:7][CH:2]([N:1]3[C:24](=[O:23])[C:19]4=[CH:18][C:17]([N+:14]([O-:16])=[O:15])=[CH:27][CH:26]=[C:20]4[C:21]3=[O:22])[CH2:3][CH2:4]2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

4

反応物 2

HCID 2309764-Nitrophthalic acid anhydrideHCID 47782391-Cyclohexylpiperidin-4-amine

生成物 1

HCID 214055491-Cyclohexyl-4-(4-nitrophthalimido)piperidine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

6.85 Grams of 4-amino-1-cyclohexylpiperidine were added to 7.26 grams of 4-nitrophthalic anhydride in 100 milliliters of chloroform and the solution was evaporated to dryness. 50 millilters of acetic anhydride were then added and the solution was heated on a steam bath for half an hour. The excess acetic anhydride was evaporated off and the residue dissolved in 40 millilters of isopropyl alcohol and the product crystallised out. This was filtered, dried and dissolved in the least amount of ethanol and ethereal hydrogen chloride added to give 2.85 grams of the title compound which was collected as the monohydrochloride. Melting Point: 265°-270° C.

後処理

  1. customthe solution was evaporated to dryness
  2. addition50 millilters of acetic anhydride were then added
  3. temperaturethe solution was heated on a steam bath for half an hour
  4. customThe excess acetic anhydride was evaporated off
  5. dissolutionthe residue dissolved in 40 millilters of isopropyl alcohol
  6. customthe product crystallised out
  7. filtrationThis was filtered
  8. customdried
  9. dissolutiondissolved in the least amount of ethanol and ethereal hydrogen chloride
  10. additionadded

出典と根拠

ORDレコード
ord-773fa9ea11ee4dd8a10393da312b47f3
出典データセット
uspto-grants-1977_10
特許番号
US04053615

反応ノート

読み込み中…