2-(4-Chlorophenoxy)ethylamine → Ethyl{[({2-[(4-chlorophenyl)oxy]ethyl}-amino)carbonyl]oxy}acetate

HRID 912727노트

반응식

HRID 912727 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH2:10][NH2:11])=[CH:4][CH:3]=1.C1([O:18][C:19]([O:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24])=O)C=CC=CC=1>C1(C)C=CC=CC=1>[CH2:26]([O:25][C:23](=[O:24])[CH2:22][O:21][C:19]([NH:11][CH2:10][CH2:9][O:8][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=1)=[O:18])[CH3:27]

참가 물질

4

반응물 2

HCID 27941912-(4-Chlorophenoxy)ethylamineHCID 12094709Ethyl [(phenoxycarbonyl)oxy]acetate

생성물 1

HCID 91288841Ethyl{[({2-[(4-chlorophenyl)oxy]ethyl}-amino)carbonyl]oxy}acetate

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A solution of 0.6 g (3.5 mmol) of [(4-chloro-phenyl)oxy]ethylamine (Chim. Ther. 1973, 8, 259-270) and 1.3 g (5.8 mmol) of ethyl [(phenyloxy-carbonyl)oxy]acetate, prepared in Step 1.1., in 30 ml of toluene is heated at 60° C. overnight. It is evaporated to dryness and the product is purified by chromatography on silica gel, eluting with a 30/70 mixture of ethyl acetate and cyclohexane. This gives 0.7 g of oily product, containing ˜10% of cyclized oxazolidine dione product, used as it is in the following step.

후처리

  1. customIt is evaporated to dryness
  2. customthe product is purified by chromatography on silica gel
  3. washeluting with a 30/70 mixture of ethyl acetate and cyclohexane
  4. additionThis gives 0.7 g of oily product, containing ˜10% of cyclized oxazolidine dione product

출처 및 근거

ORD 기록
ord-6006747349f94b0faf581af136ef8438
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026258B2

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