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

HRID 1358348

反応式

HRID 1358348 の反応式
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]

参加物

5

反応物 2

HCID 219795994,6-Dichloro-5-(o-methoxyphenoxy)-2-methyl-pyrimidineHCID 131721323HCID 131721323、化合物

生成物 1

HCID 18184223HCID 18184223、化合物収率 64.8%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c067f942e3544ed5b777df1160b0b3a0
出典データセット
uspto-grants-2003_07
特許番号
US06596719B1

関連ノート

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