5-(2-(2-(Pentafluoroethoxy) tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopentane → 5-Hexyloxy-2-[4-(5-(2-(2-(pentafluoroethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)pentyloxy)phenyl]pyrimidine

HRID 582972ノート

反応式

HRID 582972 の反応式
[CH2:1]([O:7][C:8]1[CH:9]=[N:10][C:11]([C:14]2[CH:19]=[CH:18][C:17]([OH:20])=[CH:16][CH:15]=2)=[N:12][CH:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].[F:21][C:22]([F:46])([O:27][C:28]([F:45])([F:44])[C:29]([F:43])([F:42])[O:30][C:31]([F:41])([F:40])[CH2:32][O:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38]Br)[C:23]([F:26])([F:25])[F:24]>O>[CH2:1]([O:7][C:8]1[CH:13]=[N:12][C:11]([C:14]2[CH:15]=[CH:16][C:17]([O:20][CH2:38][CH2:37][CH2:36][CH2:35][CH2:34][O:33][CH2:32][C:31]([O:30][C:29]([F:42])([F:43])[C:28]([F:44])([F:45])[O:27][C:22]([F:21])([F:46])[C:23]([F:24])([F:25])[F:26])([F:41])[F:40])=[CH:18][CH:19]=2)=[N:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

参加物

4

反応物 2

HCID 212253685-(2-(2-(Pentafluoroethoxy) tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopentaneHCID 1361744305-Hexyloxy-2-(4-hydroxyphenyl)pyrimidine

生成物 1

HCID 212253415-Hexyloxy-2-[4-(5-(2-(2-(pentafluoroethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)pentyloxy)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 5-hexyloxy-2-(4-hydroxyphenyl)pyrimidine (2.26 g, 8.3 mmol) with 5-(2(2-(pentafluoroethoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)-1-bromopentane (4.08 g, 8.3 mmol; prepared by combining 1,5-dibromopentane with 2-(2-(pentafluoroethoxy)tetrafluoroethoxy)-2,2-difluoroethanol). Product was isolated by addition of water (160 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. 190-205° C. at 0.3 torr; yield of 15.2 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. 190-205° C. at 0.3 torr; yield of 15.2 g)

出典と根拠

ORDレコード
ord-9dc70d58937443b7acb80bf238a20e17
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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