3-(2-(2-(Nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyl bromide → 4-Decyloxy-4'-(3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyloxy)tolane

HRID 583001노트

반응식

HRID 583001 반응식
[CH2:1]([O:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]#[C:19][C:20]2[CH:25]=[CH:24][C:23]([OH:26])=[CH:22][CH:21]=2)=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[F:27][C:28]([F:56])([C:52]([F:55])([F:54])[F:53])[C:29]([F:51])([F:50])[C:30]([F:49])([F:48])[O:31][C:32]([F:47])([F:46])[C:33]([F:45])([F:44])[O:34][C:35]([F:43])([F:42])[CH2:36][O:37][CH2:38][CH2:39][CH2:40]Br>>[CH2:1]([O:11][C:12]1[CH:13]=[CH:14][C:15]([C:18]#[C:19][C:20]2[CH:25]=[CH:24][C:23]([O:26][CH2:40][CH2:39][CH2:38][O:37][CH2:36][C:35]([O:34][C:33]([F:44])([F:45])[C:32]([F:46])([F:47])[O:31][C:30]([F:48])([F:49])[C:29]([F:50])([F:51])[C:28]([F:27])([F:56])[C:52]([F:55])([F:54])[F:53])([F:43])[F:42])=[CH:22][CH:21]=2)=[CH:16][CH:17]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]

참가 물질

3

반응물 2

HCID 218324923-(2-(2-(Nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyl bromideHCID 675816684-{[4-(Decyloxy)phenyl]ethynyl}phenol

생성물 1

HCID 867543064-Decyloxy-4'-(3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyloxy)tolane

실험 절차

The title compound was prepared essentially as in Example 1 by combining 4-decyloxy-4'-hydroxytolane (1.5 g, 4.3 mmol, prepared essentially as described in EP 641850) with 3-(2-(2-(nonafluorobutoxy)tetrafluoroethoxy)-2,2-difluoroethoxy)propyl bromide (2.6 g, 4.7 mmol). The reaction mixture was quenched with water, and the resulting crude product was further purified by recrystallization from ethanol, followed by Kugelrohr distillation (200-220° C. at 0.5 torr), to provide a yield of 2.64 g.

후처리

  1. customprepared essentially
  2. customThe reaction mixture was quenched with water
  3. customthe resulting crude product was further purified by recrystallization from ethanol
  4. distillationfollowed by Kugelrohr distillation (200-220° C. at 0.5 torr)
  5. customto provide a yield of 2.64 g

출처 및 근거

ORD 기록
ord-febb62542f0a4517b0c06e280eee1265
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05928562

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