4,6-Dichloro-5-(o-methoxyphenoxy)-2-methyl-pyrimidine → HCID 18184223, 화합물

HRID 1358348

반응식

HRID 1358348 반응식
Cl[C:2]1[C:7]([O:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[O:15][CH3:16])=[C:6]([Cl:17])[N:5]=[C:4]([CH3:18])[N:3]=1.[K+].[C:20]([C:24]1[CH:29]=[CH:28][C:27]([S:30]([NH-:33])(=[O:32])=[O:31])=[CH:26][CH:25]=1)([CH3:23])([CH3:22])[CH3:21]>CS(C)=O.O>[C:20]([C:24]1[CH:29]=[CH:28][C:27]([S:30]([NH:33][C:2]2[C:7]([O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[O:15][CH3:16])=[C:6]([Cl:17])[N:5]=[C:4]([CH3:18])[N:3]=2)(=[O:31])=[O:32])=[CH:26][CH:25]=1)([CH3:23])([CH3:21])[CH3:22]

참가 물질

5

반응물 2

HCID 219795994,6-Dichloro-5-(o-methoxyphenoxy)-2-methyl-pyrimidineHCID 131721323HCID 131721323, 화합물

생성물 1

HCID 18184223HCID 18184223, 화합물수율 64.8%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

To a solution of 1.0 g of 4,6-dichloro-5-(o-methoxyphenoxy)-2-methyl-pyrimidine in 20 ml of DMSO was added 1.76 g of 4-tert.-butyl-benzene sulfonamide potassium salt. The mixture was stirred for 72 h at room temperature. The solution was diluted with 250 ml of water and extracted twice with 200 ml of diehtyl ether. The organic layers were extracted twice with water. The combined aqueous layers were acidified to pH 4 with 5 ml of acetic acid and cooled to 0° C. The precipitated product was filtered off and dried in vacuo to give 1.05 g of 4-tert.-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-methyl-4-pyrimidinyl]-benzene sulfonamide as a pale beige powder. LC-MS: tR=5.64 min, [M+1]+=462.51, [M−1]−=460.63.

후처리

  1. extractionextracted twice with 200 ml of diehtyl ether
  2. extractionThe organic layers were extracted twice with water
  3. temperaturecooled to 0° C
  4. filtrationThe precipitated product was filtered off
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-c067f942e3544ed5b777df1160b0b3a0
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06596719B1

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