Methyl iodide → HCID 20272630、化合物

HRID 371368

反応式

HRID 371368 の反応式
[CH2:1]([Mg]Cl)C(C)C.C(Cl)C(C)C.[Mg].[F:13][C:14]([F:26])([F:25])[CH:15]([OH:24])[C:16]#[C:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.CI>CCOCC.[CH-]1[C-]=[C-][C-]=[C-]1.[CH-]1[C-]=[C-][C-]=[C-]1.Cl[Ti]Cl>[F:13][C:14]([F:25])([F:26])[CH:15]([OH:24])/[CH:16]=[C:17](\[C:18]1[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=1)/[CH3:1]

参加物

8

反応物 5

HCID 6328Methyl iodideHCID 10554Isobutyl chlorideHCID 5462224MagnesiumHCID 114129783-Butyn-2-ol, 1,1,1-trifluoro-4-phenyl-HCID 178418368HCID 178418368、化合物

生成物 1

HCID 20272630HCID 20272630、化合物収率 63%

試薬・触媒・溶媒 2

HCID 416358Bis(cyclopentadienyl)titanium(IV) chloride触媒HCID 3283Diethyl Ether溶媒

実験手順

In an isobutylmagnesium chloride solution that was prepared by reacting isobutyl chloride (3.74 g, 40 mmol) and magnesium (0.97 g, 40 mmol) in dry ether (40 ml) at 0° C., dichlorobis(π-cyclopentadienyl)titanium (0.22 g, 0.9 mmol) and 1,1,1-trifluoro-4-phenyl-3-butyne-2-ol (2 g, 10 mmol) were slowly added at 0° C. After 4 hour agitation of the mixture at room temperature, solvent was removed under heating for 30 min. Next, dry tetrahydrofuran (20 ml) was put into the reaction vessel and further methyl iodide (12.7 g, 90 mmol) was slowly added. After 12 hour agitation, the reaction mixture was treated by a method similar to the one in the above Examples to obtain (Z)-1,1,1-trifluoro-4-phenyl-3-pentene-2-ol (b.p.: 84°-86° C./2 mmHg) at a yield of 63%. The above product gave the following analytical data:

後処理

  1. customat 0° C.
  2. customsolvent was removed
  3. temperatureunder heating for 30 min
  4. additionwas slowly added
  5. waitAfter 12 hour agitation

出典と根拠

ORDレコード
ord-c7b863e996644d2aa218b8222f6844f3
出典データセット
uspto-grants-1985_07
特許番号
US04532020

関連ノート

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