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Acetic Anhydride → HCID 10136159、化合物

HRID 2380722
ノート
印刷プレビュー

反応式

HRID 2380722 の反応式
[C:1](OC(=O)C)(=[O:3])[CH3:2].[CH3:8][C:9]1[CH:10]=[C:11]([CH:17]2[C:21]3[CH:22]=[C:23]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:24]=[C:25]([C:26]([CH3:29])([CH3:28])[CH3:27])[C:20]=3[O:19][C:18]2=[O:34])[CH:12]=[C:13]([CH3:16])[C:14]=1[OH:15]>C1(C)C(C)=CC=CC=1.CS(O)(=O)=O>[C:1]([O:15][C:14]1[C:13]([CH3:16])=[CH:12][C:11]([CH:17]2[C:21]3[CH:22]=[C:23]([C:30]([CH3:33])([CH3:32])[CH3:31])[CH:24]=[C:25]([C:26]([CH3:27])([CH3:28])[CH3:29])[C:20]=3[O:19][C:18]2=[O:34])=[CH:10][C:9]=1[CH3:8])(=[O:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 7918Acetic AnhydrideHCID 111006493-(4-Hydroxy-3,5-dimethylphenyl)-5,7-bis(2-methyl-2-propanyl)-1-benzofuran-2(3H)-one2 回

生成物 1

HCID 10136159HCID 10136159、化合物収率 97%

試薬・触媒・溶媒 2

HCID 6395Methanesulfonic Acid触媒HCID 7237O-Xylene溶媒

反応条件

温度
105 °C

実験手順

53.6 g (0.53 mol) of acetic anhydride are added dropwise over a period of about 10 minutes to a suspension of 183.3 g (0.50 mol) of 3-(3,5-dimethyl-4-hydroxyphenyl)-5,7-di-tert-butylbenzofuran-2-one (compound (107), Table 1, Example 2) in 250 ml of xylene and 0.5 ml (7.7 mmol) of methanesulfonic acid which is stirred at 105° C. under a nitrogen atmosphere. The clear, colourless reaction mixture is concentrated at about 170° C. under a slight vacuum. 500 ml of 1-butanol are carefully added to the residue and the mixture is cooled with ice/water. The precipitated product is filtered and washed with 100 ml of 1-butanol. Drying gives 197.6 g (97%) of 3-(4-acetoxy-3,5-dimethylphenyl)-5,7-di-tert-butylbenzofuran-2-one, melting point 165°-166° C. (compound (109), Table 1).

後処理

  1. concentrationThe clear, colourless reaction mixture is concentrated at about 170° C. under a slight vacuum
  2. addition500 ml of 1-butanol are carefully added to the residue
  3. temperaturethe mixture is cooled with ice/water
  4. filtrationThe precipitated product is filtered
  5. washwashed with 100 ml of 1-butanol
  6. customDrying

出典と根拠

ORDレコード
ord-ff688b1cc3ad401dba0e20b8a8f25ae6
出典データセット
uspto-grants-1994_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05369159

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート