Acetic Anhydride → HCID 9865661、化合物

HRID 1589697ノート

反応式

HRID 1589697 の反応式
[OH:1][C:2]1[C:3]([CH3:26])=[C:4]2[C:9](=[C:10]([CH3:13])[C:11]=1[CH3:12])[O:8][C:7]([CH3:25])([CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=1)[CH2:6][CH2:5]2.[C:27](OC(=O)C)(=[O:29])[CH3:28]>N1C=CC=CC=1>[C:27]([O:1][C:2]1[C:3]([CH3:26])=[C:4]2[C:9](=[C:10]([CH3:13])[C:11]=1[CH3:12])[O:8][C:7]([CH3:25])([CH2:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][CH:17]=1)[CH2:6][CH2:5]2)(=[O:29])[CH3:28]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 134888696-Hydroxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman

生成物 1

HCID 9865661HCID 9865661、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

20.4 g of 6-hydroxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman were dissolved in 60 ml of pyridine, and, while stirring, 30 ml of acetic anhydride were added dropwise at 10° C. The mixture was gradually restored to room temperature and then reacted for 1 hour at 30° C. The reaction mixture was cooled and then poured into ice-water and extracted with a 1:1 by volume mixture of benzene and cyclohexane. The extract was washed well with a 2% w/v aqueous solution of hydrochloric acid and then with water, after which it was dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure, giving the desired 6-acetoxy-2,5,7,8-tetramethyl-2-(4-nitrophenoxymethyl)chroman. Rf value on thin layer chromatography: 0.64 [silica gel; developing solvent; benzene and ethyl acetate=10:1 by volume]

後処理

  1. customwas gradually restored to room temperature
  2. customreacted for 1 hour at 30° C
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with a 1:1 by volume mixture of benzene and cyclohexane
  5. washThe extract was washed well with a 2% w/v aqueous solution of hydrochloric acid
  6. dry with materialwith water, after which it was dried over anhydrous sodium sulfate
  7. customThe solvent was removed by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-852bfe20320d4c469e74b5bdcfdeb0de
出典データセット
uspto-grants-1986_02
特許番号
US04572912

反応ノート

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