Acetic Anhydride → HCID 57772117, 화합물

HRID 2405185노트

반응식

HRID 2405185 반응식
[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]

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 17604238HCID 17604238, 화합물

생성물 1

HCID 57772117HCID 57772117, 화합물수율 64%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-85d3a7403eb54e45b0dc9c5923283745
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802892B2

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