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Hydrogen Peroxide → 3-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-benzyloxybenzoic Acid

HRID 1830223
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인쇄 미리보기

반응식

HRID 1830223 반응식
P([O-])(O)(O)=O.[Na+].Cl([O-])=O.[Na+].[OH:11]O.[CH3:13][O:14][C:15]1[C:16]([CH3:44])=[C:17]([C:35]([O:42][CH3:43])=[C:36]([O:40][CH3:41])[C:37]=1[O:38][CH3:39])[CH2:18][C:19]1[C:20]([O:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[C:21]([CH:24]=[CH:25][CH:26]=1)[CH:22]=[O:23]>O.C(#N)C>[CH3:13][O:14][C:15]1[C:16]([CH3:44])=[C:17]([C:35]([O:42][CH3:43])=[C:36]([O:40][CH3:41])[C:37]=1[O:38][CH3:39])[CH2:18][C:19]1[C:20]([O:27][CH2:28][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[C:21]([CH:24]=[CH:25][CH:26]=1)[C:22]([OH:11])=[O:23]
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참가 물질

7

반응물 4

HCID 784Hydrogen PeroxideHCID 21919151HCID 21919151, 화합물HCID 23668197Sodium ChloriteHCID 23672064Monosodium phosphate

생성물 1

HCID 219192093-(3,4,5,6-Tetramethoxy-2-methylbenzyl)-2-benzyloxybenzoic Acid수율 98%

시약·촉매·용매 2

HCID 962
Water
용매
HCID 6342Acetonitrile용매

실험 절차

An aqueous solution (7 ml) of sodium dihydrogenphosphate (4.01 g, 33.42 mmol), an aqueous solution (7 ml) of sodium chlorite (1.74 g, 19.33 mmol) and aqueous hydrogen peroxide (1.89 ml, 30%) were added to an acetonitrile solution (12 ml) of 3-(3,4,5,6-tetramethoxy-2-methylbenzyl)-2-benzyloxybenzaldehyde (1.87 g, 4.28 mmol) and the resulting solution was stirred at room temperature for 5 hours. The reaction solution was diluted with water and then extracted with ethyl acetate. The extract was washed with an aqueous saturated sodium hydrosulfite (Na2S2O4) solution and saturated brine, then dried and concentrated to obtain the titled compound (1.90 g, 4.20 mmol, 98%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with an aqueous saturated sodium hydrosulfite (Na2S2O4) solution and saturated brine
  3. customdried
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-47f1811f559147b8a08da6acbde6bdd2
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07064124B2

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