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Water → HCID 10171447, 화합물

HRID 1768446
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HRID 1768446 반응식
[CH3:1][C:2]1([CH3:17])[C:10]2[C:5](=[CH:6][C:7]([CH3:16])=[C:8]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH:9]=2)[CH2:4][CH2:3]1.O=O.O.C([O:25]C)(C)(C)C>C(O)(=O)C>[CH3:17][C:2]1([CH3:1])[C:10]2[C:5](=[CH:6][C:7]([CH3:16])=[C:8]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])[CH:9]=2)[C:4](=[O:25])[CH2:3]1
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참가 물질

6

반응물 4

HCID 962WaterHCID 977OxygenHCID 15413tert-Butyl methyl etherHCID 113337443,3,6-Trimethyl-5-butoxy-indane

생성물 1

HCID 10171447HCID 10171447, 화합물수율 75.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
40 °C

실험 절차

100 g 3,3,6-trimethyl-5-butoxy-indane are dissolved in 400 g acetic acid and 1 g Co-II acetate is added. The reaction mixture is heated to 40° C., with stirring, and oxygen is passed through this solution for 10 hours. After cooling to room temperature, 500 g water and 500 g methyl tert.-butyl ether are added. After phase separation, the organic phase is rinsed with a further 200 g water and distilled in a 30 cm packed column. 80 g 3,3,6-trimethyl-5-butoxy-indan-1-one is obtained, which corresponds to a yield of 75% of theory. The compound can be recrystallised from heptane and a white solid is obtained, melting point: 59° C.

후처리

  1. temperatureAfter cooling to room temperature
  2. customAfter phase separation
  3. washthe organic phase is rinsed with a further 200 g water
  4. distillationdistilled in a 30 cm

출처 및 근거

ORD 기록
ord-e95ca16bb51042ed9e3faaea669f8e17
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07235699B2

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