Methanesulfonamide, N-(aminosulfonyl)-N-methyl- → 1-[(N-Methylsulfonyl-N-methylamino)sulfonyl]-3-(4-methoxy-6-methyl-2-pyrimidyl)urea

HRID 466255

반응식

HRID 466255 반응식
[CH3:1][S:2]([N:5]([S:7]([NH2:10])(=[O:9])=[O:8])[CH3:6])(=[O:4])=[O:3].[CH3:11][O:12][C:13]1[CH:18]=[C:17]([CH3:19])[N:16]=[C:15]([NH:20][C:21](=O)[O:22]C2C=CC=CC=2)[N:14]=1>ClC1C=CC=CC=1>[CH3:1][S:2]([N:5]([S:7]([NH:10][C:21]([NH:20][C:15]1[N:14]=[C:13]([O:12][CH3:11])[CH:18]=[C:17]([CH3:19])[N:16]=1)=[O:22])(=[O:9])=[O:8])[CH3:6])(=[O:4])=[O:3]

참가 물질

4

반응물 2

HCID 11084607Methanesulfonamide, N-(aminosulfonyl)-N-methyl-HCID 13577349Phenyl (4-methoxy-6-methylpyrimidin-2-yl)carbamate

생성물 1

HCID 133717831-[(N-Methylsulfonyl-N-methylamino)sulfonyl]-3-(4-methoxy-6-methyl-2-pyrimidyl)urea수율 96.4%

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

반응 조건

온도
100 °C

실험 절차

37.6 g of (N-methylsulfonyl-N-methylamino)sulfonamide are dissolved in 500 ml of chlorobenzene, 51.8 g of phenyl 4-methoxy-6-methyl-2-pyrimidylcarbamate are added dropwise at room temperature to the solution, and the mixture is stirred for 5 hours at 100° C. The mixture is cooled to 0° C., the precipitate is then filtered off, and, after washing with 100 ml of chlorobenzene, 68.8 g of the desired product of a purity of 98.7% are obtained. This corresponds to a yield of 96.4% of theory. The melting point of the product is 118-120° C.

후처리

  1. temperatureThe mixture is cooled to 0° C.
  2. filtrationthe precipitate is then filtered off
  3. washafter washing with 100 ml of chlorobenzene, 68.8 g of the desired product of a purity of 98.7%
  4. customare obtained
  5. customis 118-120° C.

출처 및 근거

ORD 기록
ord-55bb1e8f570f42b7b39a2ad831b1a37b
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05155222

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