Methyl Ethyl Ketone → HCID 23333251, 화합물

HRID 224471

반응식

HRID 224471 반응식
[CH3:1][C:2]1[CH:8]=[C:7]([OH:9])[C:6]([C:10](=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])=[CH:5][C:3]=1[OH:4].C(=O)([O-])[O-].[K+].[K+].[CH2:33]([C:35](C)=O)[CH3:34].C(Br)C=C>O>[CH2:35]([O:4][C:3]1[CH:5]=[C:6]([C:10](=[O:26])[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:7]([OH:9])=[CH:8][C:2]=1[CH3:1])[CH:33]=[CH2:34]

참가 물질

6

반응물 4

HCID 6569Methyl Ethyl KetoneHCID 7841Allyl bromideHCID 11430Potassium CarbonateHCID 147165312-Methyl-5-hexadecanoylhydroquinone

생성물 1

HCID 23333251HCID 23333251, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Under nitrogen atmosphere a mixture of 17.5 g of the keto-compound of step 1, 10.2 g of potassium carbonate and 200 ml of methyl ethyl ketone was refluxed with stirring together with 6.9 g of allyl bromide for 1 hour. After a total refluxing time of 9 h the reaction mixture was mixed with 100 ml of water. The methyl ethyl ketone layer is separated, shaken twice with a 20% by weight sodium chloride solution and dried with sodium sulphate. The residue left after evaporation of the solvent was stirred with methanol, whereupon the precipitate formed was filtered with suction and recrystallized from methanol.

후처리

  1. temperaturewas refluxed
  2. customThe methyl ethyl ketone layer is separated
  3. dry with materialdried with sodium sulphate
  4. waitThe residue left
  5. customafter evaporation of the solvent
  6. stirringwas stirred with methanol, whereupon the precipitate
  7. customformed
  8. filtrationwas filtered with suction
  9. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-2d82cbf723b74eba9546114ca420b46a
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04232107

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