Ethanolamine → (+/-)-N-Hydroxyethyl-2-[4-(4-chlorophenoxy)-phenoxy]-1-propylamine hydrochloride

HRID 263083노트

반응식

HRID 263083 반응식
S(O[CH2:6][CH:7]([O:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]2[CH:22]=[CH:21][C:20]([Cl:23])=[CH:19][CH:18]=2)=[CH:12][CH:11]=1)[CH3:8])(=O)(=O)C.[NH2:24][CH2:25][CH2:26][OH:27]>O>[ClH:23].[OH:27][CH2:26][CH2:25][NH:24][CH2:6][CH:7]([O:9][C:10]1[CH:11]=[CH:12][C:13]([O:16][C:17]2[CH:18]=[CH:19][C:20]([Cl:23])=[CH:21][CH:22]=2)=[CH:14][CH:15]=1)[CH3:8]

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 21318102(+/-)-2-[4-(4-Chlorophenoxy)-phenoxyl]-propyl mesylate

생성물 1

HCID 21318077(+/-)-N-Hydroxyethyl-2-[4-(4-chlorophenoxy)-phenoxy]-1-propylamine hydrochloride

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of 10 g (0.028 mol) of the mesylate of Example 34 and of 17 g (0.280 mol) of 2-aminoethanol is slowly heated to 170° C. The reaction mixture is allowed to return to ambient temperature and is taken up in water. After extracting the insoluble matter with diethyl ether, washing the organic phase with water and drying it over dry sodium sulphate, 8.7 g of a pale yellow oil are obtained after evaporation of the solvent. 8.4 g of this product, in ethyl acetate, are treated with a solution of hydrogen chloride in ether and the product is then purified by crystallisation from a mixture of ethyl acetate and anhydrous ethanol (7:2 by volume) to give 8.3 g of white flakes which are soluble in water to the extent of 200 g/l.

후처리

  1. customto return to ambient temperature
  2. extractionAfter extracting the insoluble matter with diethyl ether
  3. washwashing the organic phase with water
  4. dry with materialdrying it over dry sodium sulphate, 8.7 g of a pale yellow oil
  5. customare obtained
  6. customafter evaporation of the solvent
  7. addition8.4 g of this product, in ethyl acetate, are treated with a solution of hydrogen chloride in ether
  8. customthe product is then purified by crystallisation from a mixture of ethyl acetate and anhydrous ethanol (7:2 by volume)
  9. customto give 8.3 g of white flakes which

출처 및 근거

ORD 기록
ord-2c76e7728b3848058b1fb19df9af6f84
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04156011

반응 노트

불러오는 중…