HCID 13075762、化合物 → N-(alpha-cyanofurfuryl)-3-methylisothiazole-4-carboxylic acid amide

HRID 1111403ノート

反応式

HRID 1111403 の反応式
Cl.[O:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[CH:7]([NH2:10])[C:8]#[N:9].[CH3:11][C:12]1[C:16]([C:17](Cl)=[O:18])=[CH:15][S:14][N:13]=1>N1C=CC=CC=1>[C:8]([CH:7]([NH:10][C:17]([C:16]1[C:12]([CH3:11])=[N:13][S:14][CH:15]=1)=[O:18])[C:3]1[O:2][CH:6]=[CH:5][CH:4]=1)#[N:9]

参加物

4

反応物 2

HCID 13075762HCID 13075762、化合物HCID 140880593-Methylisothiazole-4-carboxylic acid chloride

生成物 1

HCID 14624282N-(alpha-cyanofurfuryl)-3-methylisothiazole-4-carboxylic acid amide

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

1.2 g of alpha-(2-furyl)-alpha-aminoacetonitrile hydrochloride was dissolved in 10 ml of pyridine, and with stirring at room temperature, 1.1 g of 3-methylisothiazole-4-carboxylic acid chloride was added dropwise. After the dropwise addition, the mixture was stirred for 1 hour, and distilled under reduced pressure to remove pyridine. The residue was dissolved in ethyl acetate, separated, washed with water, and dried over sodium sulfate. The ethyl acetate layer was distilled under reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography. Elution with benzene-ethyl acetate gave 1.2 g (yield of the desired N-(alpha-cyanofurfuryl)-3-methylisothiazole-4-carboxylic acid amide.

後処理

  1. additionAfter the dropwise addition
  2. stirringthe mixture was stirred for 1 hour
  3. distillationdistilled under reduced pressure
  4. customto remove pyridine
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. customseparated
  7. washwashed with water
  8. dry with materialdried over sodium sulfate
  9. distillationThe ethyl acetate layer was distilled under reduced pressure
  10. customto remove the solvent
  11. customThe residue was purified by silica gel column chromatography
  12. washElution with benzene-ethyl acetate

出典と根拠

ORDレコード
ord-4167489874c14e7e8e3f5ffcf089da39
出典データセット
uspto-grants-1990_12
特許番号
US04980363

反応ノート

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