Sodium hydride → 7-Fluoro-2-methyl-2,4,5,10-tetrahydropyrazolo[3,4-b][1,5]benzodiazepin-4-one

HRID 1153854노트

반응식

HRID 1153854 반응식
CS([CH2-])=O.[Na+].[H-].[Na+].[NH2:8][C:9]1[CH:26]=[C:25]([F:27])[CH:24]=[CH:23][C:10]=1[NH:11][C:12]1[C:16]([C:17](OCC)=[O:18])=[CH:15][N:14]([CH3:22])[N:13]=1>CS(C)=O>[F:27][C:25]1[CH:24]=[CH:23][C:10]2[NH:11][C:12]3=[N:13][N:14]([CH3:22])[CH:15]=[C:16]3[C:17](=[O:18])[NH:8][C:9]=2[CH:26]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 10154010Methane, sulfinylbis-, ion(1-), sodiumHCID 12888758Ethyl 3-(2-amino-4-fluoroanilino)-1-methylpyrazole-4-carboxylate

생성물 1

HCID 1357590917-Fluoro-2-methyl-2,4,5,10-tetrahydropyrazolo[3,4-b][1,5]benzodiazepin-4-one

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

반응 조건

온도
65 °C

실험 절차

A solution of sodium methyl sulphinyl methanide was generated by stirring sodium hydride (50% oil dispersion, 1.5 g) in dry dimethylsulphoxide (15 ml) at 65° C. until gas evolution ceased. A solution of ethyl 3-(2-amino-4-fluoroanilino)-1-methylpyrazole-4-carboxylate (2.7 g) dissolved in dry dimethyl sulphoxide (5 ml) was added dropwise and the mixture stirred at 65° C. for 20 minutes. The mixture was poured on to excess ice-water, filtered and dried to give the title compound which was crystallised from chloroform-hexane m.p. 264° C.

후처리

  1. additionwas added dropwise
  2. filtrationfiltered
  3. customdried

출처 및 근거

ORD 기록
ord-299f347667914d7cb98c16500adfcc49
출처 데이터셋
uspto-grants-1984_12
특허 번호
US04486591

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