3-(2-(2-(Nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyl bromide → 5-Heptyloxy-2-[4-(3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propoxy)phenyl]pyrimidine

HRID 582959ノート

反応式

HRID 582959 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[N:11][C:12]([C:15]2[CH:20]=[CH:19][C:18]([OH:21])=[CH:17][CH:16]=2)=[N:13][CH:14]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[F:22][C:23]([F:51])([C:47]([F:50])([F:49])[F:48])[C:24]([F:46])([F:45])[C:25]([F:44])([F:43])[O:26][C:27]([F:42])([F:41])[C:28]([F:40])([F:39])[O:29][C:30]([F:38])([F:37])[CH2:31][O:32][CH2:33][CH2:34][CH2:35]Br>O>[CH2:1]([O:8][C:9]1[CH:14]=[N:13][C:12]([C:15]2[CH:16]=[CH:17][C:18]([O:21][CH2:35][CH2:34][CH2:33][O:32][CH2:31][C:30]([O:29][C:28]([F:39])([F:40])[C:27]([F:41])([F:42])[O:26][C:25]([F:43])([F:44])[C:24]([F:45])([F:46])[C:23]([F:22])([F:51])[C:47]([F:50])([F:49])[F:48])([F:38])[F:37])=[CH:19][CH:20]=2)=[N:11][CH:10]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]

参加物

4

実験手順

The title compound was prepared essentially as described in Example 1 by combining 5-heptyloxy-2-(4-hydroxyphenyl)pyrimidine (3.0 g, 10.0 mmol) and 3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopropane (6.6 g, 12.0 mmol, Example 10). The product was isolated by addition of water (60 mL) to the resulting 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 Kugelrohr distillation (b.p. 180-190° C. at 2 torr; yield 5.6 g).

後処理

  1. filtrationfollowed by filtration and recrystallization from ethanol
  2. customThe recrystallized precipitate was dried at about 130° C.
  3. distillationthe resulting product was further purified by Kugelrohr distillation (b.p. 180-190° C. at 2 torr; yield 5.6 g)

出典と根拠

ORDレコード
ord-a720e0b1f2e14af1aaa5b0c2d38d8663
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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