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Pyridine → 5-bromopentyl (2Z)-4-{[tert-butyl(dimethyl)silyl]oxy}-2-[4-(methylsulfonyl)phenyl]-3-phenylbut-2-enyl carbonate

HRID 1269357
ノート
印刷プレビュー

反応式

HRID 1269357 の反応式
[Br:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][OH:7].N1C=CC=CC=1.ClC(Cl)(O[C:18](=[O:24])[O:19][C:20](Cl)(Cl)Cl)Cl.[Si:26]([O:33][CH2:34]/[C:35](/[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)=[C:36](/[C:39]1[CH:44]=[CH:43][C:42]([S:45]([CH3:48])(=[O:47])=[O:46])=[CH:41][CH:40]=1)\CO)([C:29]([CH3:32])([CH3:31])[CH3:30])([CH3:28])[CH3:27].[Cl-].[NH4+]>C(Cl)Cl>[C:18](=[O:24])([O:19][CH2:20]/[C:36](/[C:39]1[CH:44]=[CH:43][C:42]([S:45]([CH3:48])(=[O:47])=[O:46])=[CH:41][CH:40]=1)=[C:35](/[C:49]1[CH:54]=[CH:53][CH:52]=[CH:51][CH:50]=1)\[CH2:34][O:33][Si:26]([C:29]([CH3:32])([CH3:30])[CH3:31])([CH3:28])[CH3:27])[O:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][Br:1]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 1049Pyridine2 回HCID 25517Ammonium ChlorideHCID 94429TriphosgeneHCID 1187091-Pentanol, 5-bromo-HCID 58787782(2Z)-4-{[tert-butyl(dimethyl)silyl]oxy}-2-[4-(methylsulfonyl)phenyl]-3-phenylbut-2-en-1-ol

生成物 1

HCID 58841185
5-bromopentyl (2Z)-4-{[tert-butyl(dimethyl)silyl]oxy}-2-[4-(methylsulfonyl)phenyl]-3-phenylbut-2-enyl carbonate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

To a solution of 5-bromo-1-pentanol (1 eq, 0.35M) in CH2Cl2 was added pyridine (1.1 eq). The mixture was cooled at −78° C. and a solution of triphosgene (0.33 eq, 0.1M) was slowly added, the mixture was warmed to rt and stirred for 5 min. The reaction mixture was then slowly added to a mixture of (2Z)-4-{[tert-butyl(dimethyl)silyl]oxy}-2-[4-(methylsulfonyl)phenyl]-3-phenylbut-2-en-1-ol (L eq) and pyridine (1 eq) in CH2Cl (0.35M) precooled at −78° C. The reaction mixture was warmed to 0° C. and stirred 5 min. Saturated aqueous ammonium chloride was added and the mixture was extracted with EtOAc. The combined organic layers were dried over Na2SO4, filtered and concentrated. The residue was purified by flash chromatography on silica gel eluted with 1:6 to 1:1 EtOAc/hexanes to give the titled compound.

後処理

  1. temperaturethe mixture was warmed to rt
  2. customprecooled at −78° C
  3. temperatureThe reaction mixture was warmed to 0° C.
  4. stirringstirred 5 min
  5. extractionthe mixture was extracted with EtOAc
  6. dry with materialThe combined organic layers were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was purified by flash chromatography on silica gel
  10. washeluted with 1:6 to 1:1 EtOAc/hexanes

出典と根拠

ORDレコード
ord-a48737ac9e82473ba79e94eca16f836c
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07199154B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート