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Acetic Anhydride → HCID 18945439, 화합물

HRID 399827
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HRID 399827 반응식
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N:13]2[CH:17]=[CH:16][CH:15]=[CH:14]2)[CH:12]=1)[C:6]([O:8][CH3:9])=[O:7].[C:18](OC(=O)C)(=[O:20])[CH3:19]>N1C=CC=CC=1>[C:18]([O:1][CH2:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11]([N:13]2[CH:17]=[CH:16][CH:15]=[CH:14]2)[CH:12]=1)[C:6]([O:8][CH3:9])=[O:7])(=[O:20])[CH3:19]
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참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 18945167HCID 18945167, 화합물

생성물 1

HCID 18945439HCID 18945439, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

To a solution of methyl 3-hydroxymethyl-5-(pyrrol-1-yl)benzoate (4.0 g) in pyridine (40 ml) was added acetic anhydride (4.9 ml) under ice cooling. After being stirred for 3 hours under ice cooling, the reaction mixture was poured into ice-water and the product was extracted with diethyl ether. The diethyl ether extracts were washed with water, 1N-hydrochloric acid and brine and dried over magnesium sulfate. The solvent was evaporated in vacuo and the residue was purified by column chromatography on silica gel eluting with a mixture of hexane and ethyl acetate (5:1). The eluted fractions containing the desired product were collected and evaporated in vacuo to afford methyl 3-acetoxymethyl-5-(pyrrol-1-yl)benzoate (4.68 g).

후처리

  1. extractionthe product was extracted with diethyl ether
  2. washThe diethyl ether extracts were washed with water, 1N-hydrochloric acid and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was evaporated in vacuo
  5. customthe residue was purified by column chromatography on silica gel eluting with a mixture of hexane and ethyl acetate (5:1)
  6. additionThe eluted fractions containing the desired product
  7. customwere collected
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-c84d4bc6d9c44379acd7557ceb89c5ed
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05824691

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