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

HRID 2085090

반응식

HRID 2085090 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]=[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]

참가 물질

4

반응물 2

HCID 15819130HCID 15819130, 화합물HCID 1317209445-Isopropyl pyridine-2-sulfonamide potassium salt

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6dd33fb52f5a4519940194809d77d15b
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720322B2

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