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2-Methyl-2-butene → 2-(Benzyloxymethyl)-4,6-bis(methoxymethoxy)benzoic acid

HRID 505662
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HRID 505662 반응식
[CH2:1]([O:8][CH2:9][C:10]1[CH:17]=[C:16]([O:18][CH2:19][O:20][CH3:21])[CH:15]=[C:14]([O:22][CH2:23][O:24][CH3:25])[C:11]=1[CH:12]=[O:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CC(=CC)C.Cl([O-])=[O:32].[Na+].P([O-])(O)(O)=O.[Na+]>C(O)(C)(C)C.O>[CH2:1]([O:8][CH2:9][C:10]1[CH:17]=[C:16]([O:18][CH2:19][O:20][CH3:21])[CH:15]=[C:14]([O:22][CH2:23][O:24][CH3:25])[C:11]=1[C:12]([OH:32])=[O:13])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 105532-Methyl-2-buteneHCID 216698172-(Benzyloxymethyl)-4,6-bis(methoxymethoxy)benzaldehydeHCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

생성물 1

HCID 687174092-(Benzyloxymethyl)-4,6-bis(methoxymethoxy)benzoic acid수율 112.8%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6386tert-Butanol용매

실험 절차

The above-obtained 2-(benzyloxymethyl)-4,6-bis(methoxymethoxy)benzaldehyde (0.80 g, 2.3 mmol) was dissolved in tert-butyl alcohol (20 mL) and the obtained solution was added with 2-methyl-2-butene (10 mL, 94 mmol), sodium chlorite (2.0 g, 22 mmol), sodium dihydrogen phosphate (2.0 g, 17 mmol) and water (5 mL), followed by stirring at a room temperature for 10 hours. The reaction mixture was extracted with chloroform 3 times. The organic layers were combined, washed with saturated brine, dried over anhydrous sodium sulfate. Then the solvent was evaporated under reduced pressure to obtain 2-(benzyloxymethyl)-4,6-bis(methoxymethoxy)benzoic acid (0.94 g, 100%).

후처리

  1. extractionThe reaction mixture was extracted with chloroform 3 times
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThen the solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-acfebf0766b54e6a9f1d4344baad0be6
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781485B2

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