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Formic Acid → 7-sec.Butylamino-5-methylthiazolo[5,4-b]pyridine-6-carboxylic acid, ethyl ester

HRID 1606542
ノート
印刷プレビュー

反応式

HRID 1606542 の反応式
[NH2:1][C:2]1[C:3]([NH:15][CH:16]([CH2:18][CH3:19])[CH3:17])=[C:4]([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:5]([CH3:9])=[N:6][C:7]=1[SH:8].[CH:20](O)=O>>[CH:16]([NH:15][C:3]1[C:4]([C:10]([O:12][CH2:13][CH3:14])=[O:11])=[C:5]([CH3:9])[N:6]=[C:7]2[S:8][CH:20]=[N:1][C:2]=12)([CH2:18][CH3:19])[CH3:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 284Formic AcidHCID 178469256HCID 178469256、化合物

生成物 1

HCID 1317101617-sec.Butylamino-5-methylthiazolo[5,4-b]pyridine-6-carboxylic acid, ethyl ester

実験手順

2.8 g. of 5-amino-4-sec.butylamino-6-mercapto-2-methylpyridine-3-carboxylic acid, ethyl ester are refluxed in 10 ml. of formic acid for 12 hours. After this time, the excess acid is removed in vacuo and the residue is dissolved in 10 ml. of water. The aqueous solution is made alkaline with sodium hydroxide and extracted twice, each time with 10 ml. of ether. The ether layer is collected, dried over calcium chloride and evaporated to dryness. The residue, 7-sec.butylamino-5-methylthiazolo[5,4-b]pyridine-6-carboxylic acid, ethyl ester is distilled in vacuo, b. p.0.01 180°-185°, yield 1.8 g. (62%).

後処理

  1. customAfter this time, the excess acid is removed in vacuo
  2. dissolutionthe residue is dissolved in 10 ml
  3. extraction
extracted twice
  • customThe ether layer is collected
  • dry with materialdried over calcium chloride
  • customevaporated to dryness
  • distillationThe residue, 7-sec.butylamino-5-methylthiazolo[5,4-b]pyridine-6-carboxylic acid, ethyl ester is distilled in vacuo, b
  • customp.0.01 180°-185°, yield 1.8 g
  • 出典と根拠

    ORDレコード
    ord-a7f7e2fe2a4d46088c97e6cf0ae9278b
    出典データセット
    uspto-grants-1976_04
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US03953461

    反応ノート

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