HCID 53980706, 화합물 → 60201-60-7

HRID 1679672노트

반응식

HRID 1679672 반응식
Cl[CH2:2][CH2:3][NH:4][C:5]([N:7]([C:9]1[CH:14]=[CH:13][C:12]([C:15]([OH:24])([C:20]([F:23])([F:22])[F:21])[C:16]([F:19])([F:18])[F:17])=[CH:11][CH:10]=1)[CH3:8])=[O:6]>CO.O>[F:17][C:16]([F:19])([F:18])[C:15]([C:12]1[CH:13]=[CH:14][C:9]([N:7]([C:5]2[O:6][CH2:2][CH2:3][N:4]=2)[CH3:8])=[CH:10][CH:11]=1)([OH:24])[C:20]([F:23])([F:22])[F:21]

참가 물질

4

반응물 1

HCID 53980706HCID 53980706, 화합물

생성물 1

HCID 2131494660201-60-7수율 86.3%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

Dissolve 10.0 g (26 m. mole) of N-(2-chloroethyl)-N'-[4-(hexafluoro-2-hydroxy-2-propyl)phenyl]-N'-methyl-urea in a mixture of 50 ml of methanol and 100 ml of water. Heat for 1 hour on a steam bath. Concentrate, and partition between 1N aqueous sodium bicarbonate solution and ether (diethyl) and then extract with 200 ml of 1N hydrochloric acid. Add sodium bicarbonate and then extract with 200 ml of ether. Dry the ether extract and concentrate to obtain 7.8 g of the title compound as a white solid, m.p. 188°-190° C. The salts may be prepared by standrad techniques such as by treatment of a solution of the free base in a suitable organic solvent, e.g. ether, with the desired acid, e.g. hydrochloric, and then filtering off the precipitated salt. The hydrochloride salt melts at 147°-149° C.

후처리

  1. temperatureHeat for 1 hour on a steam bath
  2. concentrationConcentrate
  3. custompartition between 1N aqueous sodium bicarbonate solution and ether (diethyl)
  4. extractionextract with 200 ml of 1N hydrochloric acid
  5. extractionAdd sodium bicarbonate and then extract with 200 ml of ether
  6. dry with materialDry the ether
  7. extractionextract
  8. concentrationconcentrate

출처 및 근거

ORD 기록
ord-353763ece87343c9be906e14b880d9a6
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04081547

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