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

HRID 582968ノート

反応式

HRID 582968 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0ef4cc4a525c4ca1b8ed3991a25b6877
出典データセット
uspto-grants-1999_07
特許番号
US05928562

反応ノート

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