Sodium Carbonate → Ethyl (1,2-diphenylethyl)carbamate

HRID 2351103

반응식

HRID 2351103 반응식
[C:1]1([CH:7]([NH2:15])[CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(=O)([O-])[O-].[Na+].[Na+].Cl[C:23]([O:25][CH2:26][CH3:27])=[O:24]>C(Cl)Cl.O>[C:23]([NH:15][CH:7]([C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH2:8][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)([O:25][CH2:26][CH3:27])=[O:24]

참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 10928Ethyl chloroformateHCID 264821,2-Diphenylethylamine

생성물 1

HCID 234956Ethyl (1,2-diphenylethyl)carbamate

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

To a stirred two phase solution of 1,2-diphenylethylamine (30.0 g, 0.15 mol) in 300 ml of methylene chloride and 500 ml of water was added sodium carbonate (23.9 g, 0.225 mol) and the solution was cooled to 10° C. under nitrogen. Ethyl chloroformate (21.5 ml, 0.225 mol) was added dropwise over a one hour period. The reaction was warmed to ambient temperature and stirred at that temperature for 3 hours. The phases were separated and the aqueous phase was extracted with methylene chloride (75 ml). The combined methylene chloride extracts were washed with 1N HCl (200 ml), brine (200 ml), dried and evaporated to a white solid, 40.3 g. Recrystallization from cyclohexane gave N-carboethoxy-1,2-diphenylethylamine, mp 74°-75° C.

후처리

  1. temperatureThe reaction was warmed to ambient temperature
  2. customThe phases were separated
  3. extractionthe aqueous phase was extracted with methylene chloride (75 ml)
  4. washThe combined methylene chloride extracts were washed with 1N HCl (200 ml), brine (200 ml)
  5. customdried
  6. customevaporated to a white solid, 40.3 g
  7. customRecrystallization from cyclohexane

출처 및 근거

ORD 기록
ord-c83238845a544833a269c3348ebf4ddf
출처 데이터셋
uspto-grants-1989_10
특허 번호
US04871872

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