Water → 4-Methyl-piperidine-1-carboxylic Acid Methyl Ester

HRID 7213

반응식

HRID 7213 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.C(N(CC)CC)C.[CH3:15][O:16][C:17](Cl)=[O:18].O>C(Cl)Cl>[CH3:15][O:16][C:17]([N:5]1[CH2:6][CH2:7][CH:2]([CH3:1])[CH2:3][CH2:4]1)=[O:18]

참가 물질

6

반응물 4

HCID 962WaterHCID 6586Methyl chloroformateHCID 8471TriethylamineHCID 693814-Methylpiperidine

생성물 1

HCID 46431054-Methyl-piperidine-1-carboxylic Acid Methyl Ester

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a three neck round bottom flask was added 360 g of 4-methylpiperdine, 470 mL of triethylamine, and 390 mL of methylene chloride and the mixture was cooled in an ice bath. To this mixture was added methylchloroformate (260 mL) in methylene chloride (215 mL) slowly to maintain a reaction temperature of 20 C or below. The reaction was stirred overnight, then 200 mL of water was added and the layers were separated. The organic layer was washed with dilute HCl, satd. NaHCO3, and brine, and then the organic layer was dried over sodium sulfate and the solvent was removed in vacuo. The product was distilled at 90-93 C at ˜10 mm pressure to provide 338 g of product.

후처리

  1. temperaturethe mixture was cooled in an ice bath
  2. customthe layers were separated
  3. washThe organic layer was washed with dilute HCl
  4. dry with materialNaHCO3, and brine, and then the organic layer was dried over sodium sulfate
  5. customthe solvent was removed in vacuo
  6. distillationThe product was distilled at 90-93 C at ˜10 mm pressure

출처 및 근거

ORD 기록
ord-53c4bad16d5f4bd785263b5a0042463c
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084277B2

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