HCID 21556730, 화합물 → HCID 21556745, 화합물

HRID 267299노트

반응식

HRID 267299 반응식
[O-:1]I(=O)(=O)=O.[Na+].[CH3:7][S:8][C:9]1[CH:14]=[C:13]([CH:15]([CH3:17])[CH3:16])[C:12]([Br:18])=[CH:11][C:10]=1[CH:19]([CH3:21])[CH3:20]>O.CO.CC(C)=O>[CH3:7][S:8]([C:9]1[CH:14]=[C:13]([CH:15]([CH3:16])[CH3:17])[C:12]([Br:18])=[CH:11][C:10]=1[CH:19]([CH3:21])[CH3:20])=[O:1]

참가 물질

6

반응물 2

HCID 21556730HCID 21556730, 화합물HCID 23667635Sodium periodate

생성물 1

HCID 21556745HCID 21556745, 화합물

시약·촉매·용매 3

HCID 180Acetone용매HCID 887Methanol용매HCID 962Water용매

실험 절차

4-Bromo-2,5-diisopropylphenyl methyl sulfoxide was prepared as follows: A solution of 25.7 g of sodium m-periodate in 200 ml of water was added portionwise over 0.5 hour to 31.9 g of 4-bromo-2,5-diisopropylphenyl methyl sulfide (prepared in Example 1C) in 200 ml of methanol and 350 ml of acetone at ambient temperature. After stirring for 16 hours, the reaction mixture was filtered and the solid portion was extracted with chloroform. The filtrate was diluted with 1 liter of water and the solid residue that formed was collected on a filter. The second residue was extracted with chloroform. The two chloroform extracts were combined, washed with half-saturated sodium chloride solution, and dried over sodium sulfate. Removal of the chloroform gave a pale-yellow product containing some sulfide which was removed by recrystallization from n-hexane to give pure 4-bromo-2,5-diisopropylphenyl methyl sulfoxide which softened at 110°C and melted at 114°-117°C [Ʊ(S=O) 9.6μ].

후처리

  1. custom4-Bromo-2,5-diisopropylphenyl methyl sulfoxide was prepared
  2. filtrationthe reaction mixture was filtered
  3. extractionthe solid portion was extracted with chloroform
  4. additionThe filtrate was diluted with 1 liter of water
  5. customthe solid residue that formed
  6. customwas collected on a filter
  7. extractionThe second residue was extracted with chloroform
  8. washwashed with half-saturated sodium chloride solution
  9. dry with materialdried over sodium sulfate
  10. customRemoval of the chloroform
  11. customgave a pale-yellow product
  12. customwas removed by recrystallization from n-hexane

출처 및 근거

ORD 기록
ord-3e5f0e7bdda741cbbd96713499ae4618
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03941826

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