N-Methylbenzylamine → 1-Chloroethyl benzyl(methyl)carbamate

HRID 335535

반응식

HRID 335535 반응식
[CH3:1][NH:2][CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl[C:11]([O:13][CH:14]([Cl:16])[CH3:15])=[O:12]>CCOC(C)=O.C([O-])(O)=O.[Na+]>[CH2:3]([N:2]([CH3:1])[C:11](=[O:12])[O:13][CH:14]([Cl:16])[CH3:15])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

5

반응물 2

HCID 7669N-MethylbenzylamineHCID 5213051-Chloroethyl chloroformate

생성물 1

HCID 668694551-Chloroethyl benzyl(methyl)carbamate수율 54.9%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a vigorously stirred suspension of N-methylbenzylamine (0.260 mL, 2 mmol) in EtOAc (3 mL) and 3 mL of saturated NaHCO3 solution was added 1-chloroethyl chloroformate (0.160 mL, 2 mmol). Effervescence was observed. Once gas production had ceased, the reaction mixture was diluted with hexanes (10 mL). The aqueous phase was removed and the organic phase was washed with brine (5 mL), dried and concentrated to give the crude product as an oil (˜0.250 g). The compound was used in the subsequent step without further purification.

후처리

  1. customThe aqueous phase was removed
  2. washthe organic phase was washed with brine (5 mL)
  3. customdried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-ae3db1d73dcd4c48b53334174ca69ee0
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08884034B2

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