Acetic Acid → HCID 178491501、化合物

HRID 719262

反応式

HRID 719262 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:16])[CH2:12][C:13](=[O:15])[CH3:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].C(O)(=O)C.[N:21]([O-])=[O:22].[Na+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=[O:16])[C:12](=[N:21][OH:22])[C:13](=[O:15])[CH3:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 3680601-(3,4-Dimethoxyphenyl)butane-1,3-dioneHCID 23668193Sodium Nitrite

生成物 1

HCID 178491501HCID 178491501、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5 g of 1-(3,4-dimethoxyphenyl)butane-1,3-dione (41) were initially introduced into 25 ml of acetic acid, and. 1.71 g of sodium nitrite, dissolved in 5 ml of water, were then added dropwise at 15° C. The reaction solution was stirred at RT for 1 h and then remained standing for 2 h. 50 g of ice were added to the solution and the whole was then stored at 0° C. for 12 h, in connection with which the product precipitated out. The product was subsequently filtered off with suction and dried at 50° C. in a drying oven. The following was obtained: 42 C12H13NO5 (251.24); MS (ESI) 252 (M+H)

後処理

  1. additionwere then added dropwise at 15° C
  2. waitremained standing for 2 h
  3. waitthe whole was then stored at 0° C. for 12 h, in connection with which
  4. customthe product precipitated out
  5. filtrationThe product was subsequently filtered off with suction
  6. customdried at 50° C. in a drying oven
  7. customThe following was obtained

出典と根拠

ORDレコード
ord-8165c4347833472ebbe374bd2308dccc
出典データセット
uspto-grants-2006_11
特許番号
US07132428B2

関連ノート

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