Methanol → HCID 70534795、化合物

HRID 648016ノート

反応式

HRID 648016 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]([CH:9]1[N:14]2[CH:15]=[C:16]([CH3:18])[CH:17]=[C:13]2[CH:12]([C:19]([O:21]C(C)C)=[O:20])[CH2:11][CH2:10]1)=[O:8].CO.C(=O)([O-])[O-].[K+].[K+]>O>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]([CH:9]1[N:14]2[CH:15]=[C:16]([CH3:18])[CH:17]=[C:13]2[CH:12]([C:19]([OH:21])=[O:20])[CH2:11][CH2:10]1)=[O:8]

参加物

5

反応物 3

HCID 887MethanolHCID 11430Potassium CarbonateHCID 70534754HCID 70534754、化合物

生成物 1

HCID 70534795HCID 70534795、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 328 mg. of isopropyl 5-(N-methyl-2-pyrroyl)-2-methyl-5,6,7,8-tetrahydropyrrolo[1,2-a]pyridine-8-carboxylate in 5 ml. of methanol is treated with a solution of 0.28 g. of potassium carbonate in 5 ml. of water. The reaction mixture is refluxed under nitrogen atmosphere for 3 hours, cooled, and evaporated to dryness. The residue is taken up in 50 ml. of water, cooled to 0°, made acidic with 10% hydrochloric acid and the resultant mixture extracted with ethyl acetate (3×50 ml.). The combined extracts are dried over magnesium sulfate and evaporated to dryness under reduced pressure, to give 5-(N-methyl-2-pyrroyl)-2-methyl-5,6,7,8-tetrahydropyrrolo[1,2-a]pyridine-8-carboxylic acid (XIVa, R and Q=CH3, n-1).

後処理

  1. temperatureThe reaction mixture is refluxed under nitrogen atmosphere for 3 hours
  2. temperaturecooled
  3. customevaporated to dryness
  4. temperatureof water, cooled to 0°
  5. extractionthe resultant mixture extracted with ethyl acetate (3×50 ml.)
  6. dry with materialThe combined extracts are dried over magnesium sulfate
  7. customevaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-9f74e3502909454ea62c43944e3e17ba
出典データセット
uspto-grants-1983_10
特許番号
US04410534

反応ノート

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