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

HRID 848904
ノート
印刷プレビュー

反応式

HRID 848904 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7842Propargyl bromide2 回HCID 5462224MagnesiumHCID 217647851,1-Difluoro-2-hexanone

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-66596a0b9f494f59aa0c50c14313dc4c
出典データセット
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04297516

反応ノート

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