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2-Methoxypropene → 6,10,14-Trimethylpentadeca-3,5-dien-2-one

HRID 634982
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HRID 634982 반응식
[CH3:1][C:2](O)([CH2:5][CH2:6][CH2:7][CH:8]([CH3:15])[CH2:9][CH2:10][CH2:11][CH:12]([CH3:14])[CH3:13])[C:3]#[CH:4].C[O:18][C:19]([CH3:21])=[CH2:20].OS([O-])(=O)=O.[K+]>O>[CH3:1][C:2]([CH2:5][CH2:6][CH2:7][CH:8]([CH3:15])[CH2:9][CH2:10][CH2:11][CH:12]([CH3:14])[CH3:13])=[CH:3][CH:4]=[CH:20][C:19](=[O:18])[CH3:21]
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참가 물질

5

반응물 3

HCID 83002-MethoxypropeneHCID 1026523,7,11-Trimethyldodecyn-3-olHCID 516920Potassium bisulfate

생성물 1

HCID 1371016,10,14-Trimethylpentadeca-3,5-dien-2-one수율 7.3%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

190 g of 3,7,11-trimethyldodec-1-yn-3-ol (purity 95%, 0.848 mol) and 200 g of 2-methoxypropene (2.78 mol) and 0.58 g of KHSO4, dissolved in 1.74 g of water, were introduced into a pressure-resistant vessel. The reactor was flushed with nitrogen and closed. After a reaction time of 1 hour at 120° C., the mixture was cooled to about 50° C. and a further 0.58 g of KHSO4, dissolved in 1.74 g of water, was added. The mixture was once again heated to 120° C. After a reaction time of one hour, the reaction was complete. Distillation was carried out as in Example 1.147 g of a mixture comprising mainly 2-methoxypropene and 2,2-dimethoxypropane and 213 g of a fraction comprising 1.6% of 3,7,11-trimethyldodec-1-yn-3-ol, 67% of 6,10,14-trimethylpentadeca-4,5-dien-2-one, and 7.3% of 6,10,14-trimethylpentadeca-3,5-dien-2-one were obtained.

후처리

  1. additionwere introduced into a pressure-resistant vessel
  2. customThe reactor was flushed with nitrogen
  3. customclosed
  4. dissolutiona further 0.58 g of KHSO4, dissolved in 1.74 g of water
  5. additionwas added
  6. temperatureThe mixture was once again heated to 120° C
  7. customAfter a reaction time of one hour
  8. distillationDistillation

출처 및 근거

ORD 기록
ord-3df2a969f3db4b34af3d4bfafc9da65d
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06184420B2

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