Methyl iodide → HCID 20272630, 화합물

HRID 371368

반응식

HRID 371368 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 20272630HCID 20272630, 화합물수율 63%

시약·촉매·용매 2

HCID 416358Bis(cyclopentadienyl)titanium(IV) chloride촉매HCID 3283Diethyl Ether용매

실험 절차

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:

후처리

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

출처 및 근거

ORD 기록
ord-c7b863e996644d2aa218b8222f6844f3
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04532020

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