Potassium Carbonate → HCID 10619040, 화합물

HRID 1275231

반응식

HRID 1275231 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 10619040HCID 10619040, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b164e716a23b414caa2dcb6c885339f0
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06159990

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