HCID 13075762, 화합물 → N-(alpha-cyanofurfuryl)-3-methylisothiazole-4-carboxylic acid amide

HRID 1111403노트

반응식

HRID 1111403 반응식
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]

참가 물질

4

반응물 2

HCID 13075762HCID 13075762, 화합물HCID 140880593-Methylisothiazole-4-carboxylic acid chloride

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4167489874c14e7e8e3f5ffcf089da39
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04980363

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