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Water → 4-tert.-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)4-pyrimidinyl]-benzene sulfonamide

HRID 2085078
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HRID 2085078 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]([C:18]2[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=2)[N:3]=1.[K+].[C:25]([C:29]1[CH:34]=[CH:33][C:32]([S:35]([NH-:38])(=[O:37])=[O:36])=[CH:31][CH:30]=1)([CH3:28])([CH3:27])[CH3:26].O.C(OCC)C>CN(C=O)C.C(O)(=O)C>[C:25]([C:29]1[CH:34]=[CH:33][C:32]([S:35]([NH:38][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]([C:18]3[CH:23]=[CH:22][N:21]=[CH:20][CH:19]=3)[N:3]=2)(=[O:36])=[O:37])=[CH:31][CH:30]=1)([CH3:28])([CH3:26])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 962WaterHCID 3283Diethyl EtherHCID 111754584,6-Dichloro-5-(2-methoxyphenoxy)-2-(pyridin-4-YL)pyrimidineHCID 131721323HCID 131721323, 화합물

생성물 1

HCID 190957714-tert.-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)4-pyrimidinyl]-benzene sulfonamide

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 6228Dimethylformamide용매

실험 절차

To a solution of 6.1 g of 4,6-dichloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-pyrimidine (Example 1, Section a) to d)) in 100 ml of dry DMF 8.8 g of 4-tert.-butyl benzene sulfonamide potassium salt was added at room temperature. The solution was stirred over night at room temperature. The solution was added to a mixture of 150 ml of water and 100 ml of diethyl ether. The pH was adjusted to 5 by adding acetic acid. The precipitate that formed was collected, washed with water and diethyl ether. The resulting powder was suspended in boiling ethyl acetate. The mixture was allowed to cool in an icebath. Eventually, the solid material was collected and dried to yield 6.6 g of 4-tert.-butyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)4-pyrimidinyl]-benzene sulfonamide as beige crystals. LC-MS: tR=5.80 min, [M+1]+=525.31, [M−1]−=523.48.

후처리

  1. customThe precipitate that formed
  2. customwas collected
  3. washwashed with water and diethyl ether
  4. temperatureto cool in an icebath
  5. customEventually, the solid material was collected
  6. customdried

출처 및 근거

ORD 기록
ord-d41a8b84804847d8b28c5ab86cb9f656
출처 데이터셋
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06720322B2

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