Benzenesulfonamide, 3-amino- → 3-[(4-Chloropyrimidin-2-yl)amino]benzenesulfonamide

HRID 237

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HRID 237 반응식
Clc1ccnc(Cl)n1.Nc1cccc(S(N)(=O)=O)c1>C1COCCO1.CC(=O)O.CC(=O)O.CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21.O=C([O-])[O-].[Cs+].[Cs+].[Pd]>NS(=O)(=O)c1cccc(Nc2nccc(Cl)n2)c1

참가 물질

7

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온도
150 °C

실험 절차

2,4-dichloropyrimidine (200 mg, 1.34 mmol), 3-aminobenzenesulfonamide (231 mg, 1.34 mmol), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (93 mg, 0.16 mmol), cesium carbonate (875 mg, 2.68 mmol) and diacetoxypalladium (15.07 mg, 0.07 mmol) were suspended in dioxane (5 mL) and sealed into a microwave tube. The reaction was heated to 150 °C for 30 minutes in the microwave reactor and cooled to RT. The reaction mixture was diluted with EtOAc (150 mL) and washed with water (150 mL). The organic layer was dried over MgSO4, filtered and evaporated to afford crude product. The crude product was purified by flash silica chromatography, elution gradient 0 to 4% (10:1 MeOH/NH3 (aq)) in DCM. NMR analysis showed a trace amount of product.

출처 및 근거

ORD 기록
ord-07751cbdbcad4c89bdfeeea3a04ddb39
출처 데이터셋
750 AstraZeneca ELN dataset
원본 링크
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