반응식
Clc1ccnc(Nc2ccccc2)c1.NCc1ccccc1>C1CCCC1.CC(=O)N(C)C.CC(=O)O.CC(=O)O.CC(C)(C)[O-].CC(C1CCCC1P(C1CCCCC1)C1CCCCC1)P(C(C)(C)C)C(C)(C)C.[Fe].[Na+].[Pd]>c1ccc(CNc2ccnc(Nc3ccccc3)c2)cc1참가 물질
반응물 2
생성물 1
시약·촉매·용매 4
반응 조건
- 온도
- 100 °C
실험 절차
Phenylmethanamine (57.6 mg, 0.54 mmol), 4-chloro-N-phenylpyridin-2-amine (100 mg, 0.49 mmol)-diacetoxypalladium (8.78 mg, 0.04 mmol), (R)-(-)-1-[(S)-2-(DICYCLOHEXYLPHOSPHINO)FERROCENYL]ETHYLDI-T-BUTYLPHOSPHINE (32.5 mg, 0.06 mmol) and sodium 2-methylpropan-2-olate (94 mg, 0.98 mmol) were suspended in DMA (2.00 mL) and sealed into a microwave tube. The reaction was heated thermally to 100 °C for 30 minutes and cooled to RT. The reaction mixture was neutralised with HCl and purified by ion exchange chromatography, using a 20 g SCX column. The crude product was purified by preparative HPLC using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford N4-benzyl-N2-phenylpyridine-2,4-diamine (66.4 mg, 49.4 %) as an off- white solid.
출처 및 근거
- ORD 기록
- ord-101cdc30e8364adba8cbaa6b2be6e3e8
- 출처 데이터셋
- 750 AstraZeneca ELN dataset
- 원본 링크
- 출처 보기
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