Pyridine → N-(alpha-cyanofurfuryl)-3-methylisothiazole-5-carboxylic acid amide

HRID 1111404ノート

反応式

HRID 1111404 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].[OH-].[Na+].N1C=CC=CC=1.[CH3:19][C:20]1[CH:24]=[C:23]([C:25](Cl)=[O:26])[S:22][N:21]=1>C(OCC)(=O)C>[C:8]([CH:7]([NH:10][C:25]([C:23]1[S:22][N:21]=[C:20]([CH3:19])[CH:24]=1)=[O:26])[C:3]1[O:2][CH:6]=[CH:5][CH:4]=1)#[N:9]

参加物

6

反応物 4

HCID 1049PyridineHCID 14798Sodium HydroxideHCID 13075762HCID 13075762、化合物HCID 151072913-Methyl-1,2-thiazole-5-carbonyl chloride

生成物 1

HCID 14624283N-(alpha-cyanofurfuryl)-3-methylisothiazole-5-carboxylic acid amide収率 74%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

5.0 g of alpha-(2-furyl)-alpha-aminoacetonitrile hydrochloride was dehydrochlorinated with sodium hydroxide in ethyl acetate by the same method as in the above Synthesis Example 6. Pyridine (2.5 g) was added, and furthermore, an ethyl acetate solution of 4.0 g of 3-methylisothiazole-5-carboxylic acid chloride was added dropwise After the addition, the mixture was stirred for 1 hour. The reaction mixture was washed with water, dilute hydrochloric acid and a dilute aqueous solution of sodium bicarbonate. Sodium sulfate, and active carbon were added to dehydrate and decolorize the reaction mixture. The solvent was removed under reduced pressure, and the residue was washed with ethyl ether to give 4.5 g (yield 74%) of the desired N-(alpha-cyanofurfuryl)-3-methylisothiazole-5-carboxylic acid amide.

後処理

  1. additionAfter the addition
  2. washThe reaction mixture was washed with water, dilute hydrochloric acid
  3. additionSodium sulfate, and active carbon were added
  4. customThe solvent was removed under reduced pressure
  5. washthe residue was washed with ethyl ether

出典と根拠

ORDレコード
ord-6e510778c3e4480aac03312e5548e4b7
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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