HCID 15819130、化合物 → 5-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-4-pyrimidinyl]-2-pyridine sulfonamide

HRID 2085090

反応式

HRID 2085090 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]=[CH:4][N:3]=1.[K+].[CH:19]([C:22]1[CH:23]=[CH:24][C:25]([S:28]([NH-:31])(=[O:30])=[O:29])=[N:26][CH:27]=1)([CH3:21])[CH3:20]>CN(C=O)C>[CH:19]([C:22]1[CH:23]=[CH:24][C:25]([S:28]([NH:31][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]=[CH:4][N:3]=2)(=[O:30])=[O:29])=[N:26][CH:27]=1)([CH3:21])[CH3:20]

参加物

4

反応物 2

HCID 15819130HCID 15819130、化合物HCID 1317209445-Isopropyl pyridine-2-sulfonamide potassium salt

生成物 1

HCID 227294075-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-4-pyrimidinyl]-2-pyridine sulfonamide収率 64.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 2.71 g of 4,6-dichloro-5-(o-methoxyphenoxy)-pyrimidine (Example 10b) and 5.0 g of 5-isopropyl pyridine-2-sulfonamide potassium salt (Example 1e) in 50 ml of DMF was stirred at room temperature for 20 h. The solvent was removed in vacuo, the residue was taken up in 200 ml of 10% aqueous acetic acid and extracted three times with ethyl acetate. The combined organic layers were washed with water and brine, dried over MgSO4 and evaporated. The crude product was crysallised from a mixture of 2-propanol and diethyl ether. The crystals were collected, washed with cold 2-propanol and diethyl ether and dried to give 2.8 g of 5-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-4-pyrimidinyl]-2-pyridine sulfonamide as white crystals. LC-MS: tR=4.99 min, [M+1]+=435.25, [M−1]−=433.28.

後処理

  1. customThe solvent was removed in vacuo
  2. extractionextracted three times with ethyl acetate
  3. washThe combined organic layers were washed with water and brine
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. additionThe crude product was crysallised from a mixture of 2-propanol and diethyl ether
  7. customThe crystals were collected
  8. washwashed with cold 2-propanol and diethyl ether
  9. customdried

出典と根拠

ORDレコード
ord-6dd33fb52f5a4519940194809d77d15b
出典データセット
uspto-grants-2004_04
特許番号
US06720322B2

関連ノート

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