Potassium Carbonate → HCID 10619040、化合物

HRID 1275231

反応式

HRID 1275231 の反応式
[OH:1][C:2]1([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[CH2:14]([O:21][C:22]([NH:24][CH2:25][CH2:26][CH2:27]Br)=[O:23])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:14]([O:21][C:22]([NH:24][CH2:25][CH2:26][CH2:27][N:5]1[CH2:6][CH2:7][C:2]([OH:1])([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:3][CH2:4]1)=[O:23])[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 963874-Phenylpiperidin-4-olHCID 254436Benzyl 3-bromopropylcarbamate

生成物 1

HCID 10619040HCID 10619040、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 4-hydroxy-4-phenylpiperidine (5 g, 0.0282 mol), N-benzyloxycarbonyl-3-bromopropylamine (8.445 g, 0.031 mol), and potassium carbonate (7.795 g, 0.0564 mole) in acetone (200 mL) was stirred and refluxed for 12 hours. Acetone was evaporated at reduced pressure, the residue was treated with ice-cold water (400 mL) and extracted with CH2Cl2 (4×120 mL). Solvent was evaporated from the combined dried (sodium sulfate) extracts and the residue was found to be almost pure desired product (9.5 g, 91%) by tlc and 1H-NMR and was used as such without any further purification.

後処理

  1. temperaturerefluxed for 12 hours
  2. customAcetone was evaporated at reduced pressure
  3. additionthe residue was treated with ice-cold water (400 mL)
  4. extractionextracted with CH2Cl2 (4×120 mL)
  5. customSolvent was evaporated from the
  6. dry with materialcombined dried (sodium sulfate) extracts
  7. customsuch without any further purification

出典と根拠

ORDレコード
ord-b164e716a23b414caa2dcb6c885339f0
出典データセット
uspto-grants-2000_12
特許番号
US06159990

関連ノート

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