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Acetic Anhydride → HCID 18945439、化合物

HRID 399827
ノート
印刷プレビュー

反応式

HRID 399827 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 18945167HCID 18945167、化合物

生成物 1

HCID 18945439HCID 18945439、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c84d4bc6d9c44379acd7557ceb89c5ed
出典データセット
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05824691

反応ノート

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