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1,2-Epoxybutane → 3,7-Dimethyl-nona-2,4,6,8-tetraen-1-oic acid butyl ester

HRID 27849
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HRID 27849 반응식
[Cl-].Cl[C:3]1C(C)=C(C(C)=CC=1C)C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH2:32]([O:36][C:37](=[O:48])[CH:38]=[C:39]([CH3:47])[CH:40]=[CH:41][CH:42]=[C:43]([CH:45]=O)[CH3:44])[CH2:33][CH2:34][CH3:35].C1OC1CC>>[CH2:32]([O:36][C:37](=[O:48])[CH:38]=[C:39]([CH3:47])[CH:40]=[CH:41][CH:42]=[C:43]([CH3:44])[CH:45]=[CH2:3])[CH2:33][CH2:34][CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 78341,2-EpoxybutaneHCID 53845956Butyl 3,7-dimethyl-8-oxoocta-2,4,6-trienoateHCID 867358973-Chloro-2,4,6-trimethyl-benzyl-triphenylphosphonium chloride

생성물 1

HCID 542920543,7-Dimethyl-nona-2,4,6,8-tetraen-1-oic acid butyl ester

실험 절차

16 g of 3-chloro-2,4,6-trimethyl-benzyl-triphenylphosphonium chloride and 10 g of 7-formyl-3-methyl-octa-2,4,6-trien-1-oic acid butyl ester are heated to boiling with stirring after the addition of 40 g of 1,2-butylene oxide. The 1,2-butylene oxide is slowly distilled off. The reaction mixture is stirred for 30 minutes at 80°-82° C., then cooled and thoroughly extracted with hexane. The hexane extract is shaken out 5 times with 50 ml of methanol/water 70:30 parts by volume each time, then dried over sodium sulphate and evaporated under reduced pressure to produce 9-(3-chloro-2,4,6-trimethyl-phenyl), 3,7-dimethyl-nona-2,4,6,8-tetraen-1-oic acid butyl ester as a residue.

후처리

  1. distillationThe 1,2-butylene oxide is slowly distilled off
  2. stirringThe reaction mixture is stirred for 30 minutes at 80°-82° C.
  3. temperaturecooled
  4. extractionthoroughly extracted with hexane
  5. extractionThe hexane extract
  6. stirringis shaken out 5 times with 50 ml of methanol/water 70:30 parts by volume each time
  7. dry with materialdried over sodium sulphate
  8. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-5a0510b3ae024dbeafefae45eb02d3e0
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04224244

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