Hydrochloric Acid → 15-Hydroxypentadecanoic acid

HRID 1493722

반응식

HRID 1493722 반응식
[OH:1][CH2:2][CH2:3][CH2:4][C:5](=O)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17].[OH-].[K+].C(O)COCCO.Cl>O>[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8117Diethylene GlycolHCID 14797Potassium HydroxideHCID 988195515-Hydroxy-12-ketopentadecanoic acid

생성물 1

HCID 7836015-Hydroxypentadecanoic acid수율 85%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1.00 g (3.68 millimole) of 15-hydroxy-12-ketopentadecanoic acid, 0.73 g (11.0 millimole) of 85 wt.% potassium hydroxide, 0.50 g (8.5 millimole) of 85 % hydrated hydrazine and 5 ml of diethylene glycol were charged into a frask and heated under reflux over 1.5 hours. Subsequently, while evaporating the produced light boiling components such as water to the outside of the system, the internal temperature was elevated to 195 to 205° C., and the heating under reflux was continued at the same temperature range over 2 hours. After completion of the reaction, the solution was cooled, diluted by addition of 5 ml of water and added with 3 ml of 6N-HCl, followed by collection of the precipitated pail brown solid by filtration. The solid was recrystallized from benzene to obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl.

후처리

  1. temperatureheated
  2. temperatureunder reflux over 1.5 hours
  3. customSubsequently, while evaporating the produced light
  4. customwas elevated to 195 to 205° C.
  5. temperaturethe heating under reflux
  6. customAfter completion of the reaction
  7. temperaturethe solution was cooled
  8. filtrationfollowed by collection of the precipitated pail brown solid by filtration
  9. customThe solid was recrystallized from benzene
  10. customto obtain 0.81 g (3.14 millimole, Yield: 85 %) of a white crystl

출처 및 근거

ORD 기록
ord-bc798a77a48a49ffaf13ef4043394149
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05023351

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