1,5-Diazabicyclo(5,4,0)undec-5-ene → N-(3-n-butylaminopyridin-2-ylsulfonyl)-N'-(4,6-dimethoxypyrimidin-2-yl)urea

HRID 1588179노트

반응식

HRID 1588179 반응식
[CH2:1]([NH:5][C:6]1[C:7]([S:12]([NH2:15])(=[O:14])=[O:13])=[N:8][CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4].[CH3:16][O:17][C:18]1[CH:23]=[C:22]([O:24][CH3:25])[N:21]=[C:20]([NH:26][C:27](=O)[O:28]C2C=CC=CC=2)[N:19]=1.N12CCCCC1C=NCCC2>C(#N)C>[CH2:1]([NH:5][C:6]1[C:7]([S:12]([NH:15][C:27]([NH:26][C:20]2[N:19]=[C:18]([O:17][CH3:16])[CH:23]=[C:22]([O:24][CH3:25])[N:21]=2)=[O:28])(=[O:14])=[O:13])=[N:8][CH:9]=[CH:10][CH:11]=1)[CH2:2][CH2:3][CH3:4]

참가 물질

5

반응물 3

HCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 10945667Carbamic acid, N-(4,6-dimethoxy-2-pyrimidinyl)-, phenyl esterHCID 190099643-n-Butylaminopyridin-2-ylsulfonamide

생성물 1

HCID 19009965N-(3-n-butylaminopyridin-2-ylsulfonyl)-N'-(4,6-dimethoxypyrimidin-2-yl)urea

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

The following are added in succession to a mixture of 2.75 g of 3-n-butylaminopyridin-2-ylsulfonamide in 40 ml of acetonitrile: 3.5 g of phenyl N-(4,6-dimethoxypyrimidin-2-yl)carbamate and 1.97 ml of 1,5-diazabicyclo[5.4.0]undec-5-ene. The reaction mixture is stirred for 30 minutes and evaporated, the oily residue is triturated with 10 ml of 2N hydrochloric acid and subsequently with 10 ml of ice/water and a little diethyl ether, and the mixture is filtered. The filter residue is subsequently washed with a little water and diethyl ether and dried. 4.39 g of N-(3-n-butylaminopyridin-2-ylsulfonyl)-N'-(4,6-dimethoxypyrimidin-2-yl)urea (compound No. 1.001) of a melting point of 118°-119° C. are obtained.

후처리

  1. customevaporated
  2. customthe oily residue is triturated with 10 ml of 2N hydrochloric acid and subsequently with 10 ml of ice/water
  3. filtrationa little diethyl ether, and the mixture is filtered
  4. washThe filter residue is subsequently washed with a little water and diethyl ether
  5. customdried
  6. custom1.001) of a melting point of 118°-119° C. are obtained

출처 및 근거

ORD 기록
ord-d97f720ee6ba40bc94bd0ef97d7130f0
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05221315

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