Diisopropylethylamine → (R)-N,N-dimethyl-6-(methyl(1-(7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl)pyrrolidin-3-yl)amino)pyridine-3-sulfonamide

HRID 527944

反応式

Cl[C:2]1[N:7]=[CH:6][C:5]([S:8]([N:11]([CH3:13])[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1.CCN(C(C)C)C(C)C.[CH3:23][NH:24][C@@H:25]1[CH2:29][CH2:28][N:27]([C:30]2[C:31]3[CH:38]=[CH:37][N:36]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])[C:32]=3[N:33]=[CH:34][N:35]=2)[CH2:26]1>CN1C(=O)CCC1.CCOC(C)=O>[CH3:12][N:11]([CH3:13])[S:8]([C:5]1[CH:6]=[N:7][C:2]([N:24]([CH3:23])[C@@H:25]2[CH2:29][CH2:28][N:27]([C:30]3[C:31]4[CH:38]=[CH:37][N:36]([CH2:39][O:40][CH2:41][CH2:42][Si:43]([CH3:46])([CH3:45])[CH3:44])[C:32]=4[N:33]=[CH:34][N:35]=3)[CH2:26]2)=[CH:3][CH:4]=1)(=[O:10])=[O:9]

参加物

反応条件

温度: 200 °C

実験手順

To a solution of 6-chloro-N,N-dimethylpyridine-3-sulfonamide (1 mmol) and DIPEA (2.5 mmol) in NMP (2 mL) was added (R)—N-methyl-1-(7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl)pyrrolidin-3-amine (0.5 mmol). The reaction mixture was stirred at 200° C. for 60 minutes in microwave reactor. After cooling to room temperature, the mixture was diluted with EtOAc, washed with brine, dried, filtered, and concentrated. The residue was purified by chromatography with MeOH/H2O to give the title compound in yellow in 8% yield.

後処理

temperatureAfter cooling to room temperature
washwashed with brine
customdried
filtrationfiltered
concentrationconcentrated
customThe residue was purified by chromatography with MeOH/H2O

出典と根拠

ORDレコード: ord-be4699431d184566942e8e86427920cb
出典データセット: uspto-grants-2016_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09346810B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 2

反応条件

実験手順

後処理

出典と根拠

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