Acetic Anhydride → HCID 57772117、化合物

HRID 1882318ノート

反応式

HRID 1882318 の反応式
[CH3:1][O:2][C:3](=[O:16])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][OH:13])=[CH:8][C:7]=1[O:14][CH3:15].[C:17](OC(=O)C)(=[O:19])[CH3:18]>N1C=CC=CC=1>[CH3:1][O:2][C:3](=[O:16])[CH2:4][O:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][O:13][C:17](=[O:19])[CH3:18])=[CH:8][C:7]=1[O:14][CH3:15]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 17604238HCID 17604238、化合物

生成物 1

HCID 57772117HCID 57772117、化合物収率 64%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of (4-Hydroxymethyl-2-methoxy-phenoxy)-acetic acid methyl ester 72 (40 grams, 177 mmol), Acetic anhydride (80 mL) and pyridine (4 mL) was refluxed for 4 hours. Reaction mixture was poured in to ice water (200 mL) and crude 73 was extracted into chloroform, dried over Na2SO4, and distilled. The crude was vacuum distilled to give pure 73 (30 grams, 64%) as a color less liquid, Bp15 210° C. The structure was confirmed with IR and NMR. IHNMR (CDCl3) δ 2.08 (s, 3H, O═C—CH3), 3.78 (s, 3H, ester), 3.90 (s, 3H, OCH3), 4.65 (s, 2H, OCH2), 5.00 (s, 2H, CH2), 6.76 (d, 1H, Ar), 6.80 (d, 2H, Ar), 6.85 (dd, 1H, Ar).

後処理

  1. customReaction mixture
  2. extractionwas extracted into chloroform
  3. dry with materialdried over Na2SO4
  4. distillationdistilled
  5. distillationdistilled

出典と根拠

ORDレコード
ord-a22084872b4344ccba02475296d772d3
出典データセット
uspto-grants-2012_11
特許番号
US08318973B2

反応ノート

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