Hydrochloric Acid → N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea

HRID 280442노트

반응식

HRID 280442 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH3:9])[N:6]=[C:5]([N:10](C2C=CC=CC=2)[C:11](=[O:13])[O-])[N:4]=1.[N:20]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH2:32])(=[O:31])=[O:30])=[CH:25][CH:24]=1)=[N+:21]=[N-:22].N12CCCCC1C=NCCC2.Cl>O1CCOCC1.O>[N:20]([C:23]1[CH:28]=[CH:27][C:26]([S:29]([NH:32][C:11]([NH:10][C:5]2[N:4]=[C:3]([O:2][CH3:1])[CH:8]=[C:7]([CH3:9])[N:6]=2)=[O:13])(=[O:30])=[O:31])=[CH:25][CH:24]=1)=[N+:21]=[N-:22]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 35585904-AzidobenzenesulfonamideHCID 18954641N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate

생성물 1

HCID 23320462N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea수율 67%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

A solution of 2.9 g of N-(4-methoxy-6-methylpyrimidin-2-yl)phenylcarbamate in 10 ml of dioxan is added dropwise at 20°-25° C. to a solution of 2 g of 4-azidophenylsulfonamide and 1.6 ml of 1,5-diazabicyclo(5,4,0)-undec-5-ene in 20 ml of dioxan and the mixture is stirred for 3 hours at the same temperature. The reaction mixture is then taken up in 200 ml of water and the aqueous mixture is then acidified with hydrochloric acid to pH 2. The precipitated product is isolated, washed with ethyl acetate and dried, affording N-(4-azidophenylsulfonyl)-N'-(4-methoxy-6-methylpyrimidin-2-yl)urea in 67% yield in the form of greenish crystals with a melting point of 192° C.

후처리

  1. customThe precipitated product is isolated
  2. washwashed with ethyl acetate
  3. customdried

출처 및 근거

ORD 기록
ord-f5cd7d39e6fb45bea731dea7ea0ea439
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04589912

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