1-Bromo-3-chloropropane → 5-Hexyloxy-2-[4-(3-(2-(2-(trifluoromethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propoxy)phenyl]pyrimidine

HRID 2257466노트

반응식

HRID 2257466 반응식
[F:1][C:2]([F:21])([F:20])[O:3][C:4]([F:19])([F:18])[C:5]([F:17])([F:16])[O:6][C:7]([F:15])([F:14])[CH2:8][O:9][CH2:10][CH2:11][CH2:12]Cl.BrCCCCl.[CH2:27]([O:33][C:34]1[CH:35]=[N:36][C:37]([C:40]2[CH:45]=[CH:44][C:43]([OH:46])=[CH:42][CH:41]=2)=[N:38][CH:39]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]>O>[CH2:27]([O:33][C:34]1[CH:39]=[N:38][C:37]([C:40]2[CH:41]=[CH:42][C:43]([O:46][CH2:12][CH2:11][CH2:10][O:9][CH2:8][C:7]([O:6][C:5]([F:17])([F:16])[C:4]([F:19])([F:18])[O:3][C:2]([F:21])([F:20])[F:1])([F:15])[F:14])=[CH:44][CH:45]=2)=[N:36][CH:35]=1)[CH2:28][CH2:29][CH2:30][CH2:31][CH3:32]

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 212253483-(2-(2-(Trifluoromethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-chloropropaneHCID 1361744305-Hexyloxy-2-(4-hydroxyphenyl)pyrimidine

생성물 1

HCID 212253235-Hexyloxy-2-[4-(3-(2-(2-(trifluoromethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propoxy)phenyl]pyrimidine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The title compound was prepared essentially as in Example 1 by combining 3-(2-(2-(trifluoromethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-chloropropane (4.5 g, 11.7 mmol; prepared by combining 1-bromo-3-chloropropane with 3-(2-(2-(trifluoromethoxy) tetrafluoroethoxy)-2,2-difluoroethanol) with 5-hexyloxy-2-(4-hydroxyphenyl)pyrimidine (3.0 g, 11.0 mmol). The resulting product was isolated by addition of water (50 mL) to the reaction mixture, followed by filtration and recrystallization from ethanol. The recrystallized precipitate was dried at about 130° C., and the resulting product was further purified by distillation using a Kugelrohr apparatus (b.p. 180°-183° C. at 0.1 torr; yield of 3.9 g).

후처리

  1. customprepared
  2. filtrationfollowed by filtration and recrystallization from ethanol
  3. customThe recrystallized precipitate was dried at about 130° C.
  4. distillationthe resulting product was further purified by distillation

출처 및 근거

ORD 기록
ord-1422de4896974f7f8800ddcb5544d898
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05658491

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