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Methyl Isocyanate → 2,6-Diethyl-2,3,6-trimethyl-4-piperidyl methylcarbamate

HRID 616544
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HRID 616544 반응식
[CH2:1]([C:3]1([CH3:14])[CH:8]([CH3:9])[CH:7]([OH:10])[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4]1)[CH3:2].[CH3:15][N:16]=[C:17]=[O:18]>C1(C)C(C)=CC=CC=1>[CH3:15][NH:16][C:17](=[O:18])[O:10][CH:7]1[CH2:6][C:5]([CH2:12][CH3:13])([CH3:11])[NH:4][C:3]([CH2:1][CH3:2])([CH3:14])[CH:8]1[CH3:9]
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참가 물질

4

반응물 2

HCID 12228Methyl IsocyanateHCID 221822412,6-Diethyl-2,3,6-trimethylpiperidin-4-ol2회

생성물 1

HCID 537281202,6-Diethyl-2,3,6-trimethyl-4-piperidyl methylcarbamate수율 97.2%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

4.0 g of 2,6-diethyl-2,3,6-trimethyl-4-piperidinol (Compound 1) and 1.7 g of methyl isocyanate were dissolved in 6 ml of xylene and the solution was refluxed by heating for 3.5 hours. Xylene and excess methyl isocyanate were distilled off under reduced pressure. The residue was purified by column chromatography on silica gel ("60F 254", available from Merck & Co.) using a 4 : 1 by volume mixture of chloroform and methanol as eluent. The product was then distilled under reduced pressure, giving 5.0 g of Compound 66 as a pale yellow liquid (bp 145° - 149° C/1.4 mmHg).

후처리

  1. temperaturethe solution was refluxed
  2. temperatureby heating for 3.5 hours
  3. distillationXylene and excess methyl isocyanate were distilled off under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel ("60F 254", available from Merck & Co.)
  5. additionby volume mixture of chloroform and methanol as eluent
  6. distillationThe product was then distilled under reduced pressure

출처 및 근거

ORD 기록
ord-2ac982029cfd483186dcdc3096af9b37
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04075165

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