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Propargyl bromide → 4-Difluoromethyl-4-hydroxy-1-octyne

HRID 126714
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HRID 126714 반응식
[Mg].[CH2:2](Br)[C:3]#[CH:4].[F:6][CH:7]([F:14])[C:8](=[O:13])[CH2:9][CH2:10][CH2:11][CH3:12]>CCOCC>[F:6][CH:7]([F:14])[C:8]([OH:13])([CH2:9][CH2:10][CH2:11][CH3:12])[CH2:4][C:3]#[CH:2]
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참가 물질

5

반응물 3

HCID 7842Propargyl bromide2회HCID 5462224MagnesiumHCID 217647851,1-Difluoro-2-hexanone

생성물 1

HCID 127861894-Difluoromethyl-4-hydroxy-1-octyne

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

To a stirred suspension of 3.6 g. of magnesium and 30 mg. of mercuric chloride in 0.33 ml. of ether is added 1.5 ml. of propargyl bromide. The mixture is stirred vigorously for several minutes to initiate reaction, then a solution of 15.5 g. of 1,1-difluoro-2-hexanone and 12.1 ml. of propargyl bromide in 33 ml. of ether is added slowly (dropwise) over a 1.5 hour period, so that the mixture remains gently refluxing (25°-30° C.). After addition, the mixture is stirred at room temperature for 30 minutes, then cooled in an ice bath to 0°-5° C. and quenched by adding 35 ml. of saturated ammonium chloride solution dropwise and then stirred for 30 minutes. The mixture is filtered through Celite and washed with ether. The filtrate is concentrated in vacuo giving a yellow oil. This oil is vacuum distilled at 71° C., 12 mm giving the product as 10.54 g. of colorless oil which becomes pale yellow on standing at room temperature.

후처리

  1. additionTo a stirred suspension of 3.6 g
  2. customreaction
  3. temperatureso that the mixture remains gently refluxing (25°-30° C.)
  4. additionAfter addition
  5. stirringthe mixture is stirred at room temperature for 30 minutes
  6. temperaturecooled in an ice bath to 0°-5° C.
  7. customquenched
  8. additionby adding 35 ml
  9. stirringof saturated ammonium chloride solution dropwise and then stirred for 30 minutes
  10. filtrationThe mixture is filtered through Celite
  11. washwashed with ether
  12. concentrationThe filtrate is concentrated in vacuo
  13. customgiving a yellow oil
  14. distillationdistilled at 71° C.
  15. custom12 mm giving the product as 10.54 g
  16. customon standing at room temperature

출처 및 근거

ORD 기록
ord-4673685a0b594870ae155c5d289032e3
출처 데이터셋
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04254036

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