Acetic Acid → HCID 13345321、化合物

HRID 1011333ノート

反応式

HRID 1011333 の反応式
[CH3:1][C:2]1[N:7](C(O)=O)[CH:6]([C:11]([OH:13])=[O:12])[CH:5]=[CH:4][CH:3]=1.[C:14](O)(=[O:16])C.N1C=CC=CC=1.CCCCCC>COCCOC.CCOCC>[CH3:1][C:2]1[N:7]=[C:6]2[C:11](=[O:12])[O:13][C:14](=[O:16])[C:5]2=[CH:4][CH:3]=1

参加物

7

反応物 4

HCID 176Acetic AcidHCID 1049PyridineHCID 8058HexaneHCID 67315455HCID 67315455、化合物

生成物 1

HCID 13345321HCID 13345321、化合物収率 74.2%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of 6-methyl-1,2-pyridine dicarboxylic acid (25 g, 138 mmol) and acetic acid (42 mL, 733 mmol) in DME (150 mL) is treated with pyridine (22 mL, 272 mmol) and stirred at room temperature for 2 h. The pale yellow solution is diluted with ether (250 mL) and then hexane (1250 mL) is added slowly. A white precipitate is formed. The solution is cooled to 0° C. for 30 min and the white solid is collected by filtration. The solid is washed with hexane and dried to give the title compound as a white solid (16.7 g, 74%).

後処理

  1. customA white precipitate is formed
  2. temperatureThe solution is cooled to 0° C. for 30 min
  3. filtrationthe white solid is collected by filtration
  4. washThe solid is washed with hexane
  5. customdried

出典と根拠

ORDレコード
ord-0696e96a5a6847609df9f444b7c2846a
出典データセット
uspto-grants-2011_07
特許番号
US07977351B2

反応ノート

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