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1-Bromo-3,5-bis(trifluoromethyl)benzene → HCID 22721472、化合物

HRID 1581451
ノート
印刷プレビュー

反応式

HRID 1581451 の反応式
[CH3:1][C:2]1[C:11](Cl)=[C:10]([CH3:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[F:43][C:44]([F:58])([F:57])[C:45]1[CH:46]=[C:47]([Mg]Br)[CH:48]=[C:49]([C:51]([F:54])([F:53])[F:52])[CH:50]=1.FC(F)(F)C1C=C(Br)C=C(C(F)(F)F)C=1>O.C1COCC1>[CH3:1][C:2]1[C:11]([C:47]2[CH:48]=[C:49]([C:51]([F:54])([F:52])[F:53])[CH:50]=[C:45]([C:44]([F:43])([F:58])[F:57])[CH:46]=2)=[C:10]([CH3:13])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 676021-Bromo-3,5-bis(trifluoromethyl)benzeneHCID 812191,3-Bis(diphenylphosphino)propaneHCID 110846922,4-Dimethyl-3-chloroquinolineHCID 178506227HCID 178506227、化合物

生成物 1

HCID 22721472HCID 22721472、化合物

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a THF solution of the obtained 2,4-dimethyl-3-chloroquinoline (0.65 g) and Ni(dpp)Cl2 (dpp: 1,3-bis(diphenylphosphino)propane) (0.1 g), 3,5-bis (trifluoromethyl)phenylmagnesium bromide prepared from Mg and 3,5-bis(trifluoromethyl)bromobenzene was dropped and the reaction solution was allowed to react for 24 hours at room temperature. Water was added to the reaction solution and the organic layer was extracted using CHCl3. The solvent was removed under reduced pressure and the residue was purified through column chromatography to obtain 2,4-dimethyl-3-[3,5-bis(trifluoromethyl)phenyl]quinoline.

後処理

  1. additionwas dropped
  2. customto react for 24 hours at room temperature
  3. extractionthe organic layer was extracted
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified through column chromatography

出典と根拠

ORDレコード
ord-ea8b7a32c1914b7a8f7b9eeebab843de
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06730418B2

反応ノート

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