Bromotrimethylsilane → HCID 178485575、化合物

HRID 2279887ノート

反応式

HRID 2279887 の反応式
[Br:1][C:2]1[N:7]=[C:6]([C:8](=[O:11])[NH:9][CH3:10])[C:5]([NH:12][C:13]2[C:18]([C:19]([F:22])([F:21])[F:20])=[CH:17][N:16]=[C:15]([NH:23][C:24]3[CH:34]=[CH:33][C:27]([CH2:28][CH2:29][PH:30](=[O:32])[O-:31])=[CH:26][C:25]=3[O:35][CH3:36])[N:14]=2)=[CH:4][CH:3]=1.Br[Si](C)(C)C>N1C=CC=CC=1>[Br:1][C:2]1[N:7]=[C:6]([C:8](=[O:11])[NH:9][CH3:10])[C:5]([NH:12][C:13]2[C:18]([C:19]([F:22])([F:20])[F:21])=[CH:17][N:16]=[C:15]([NH:23][C:24]3[CH:34]=[CH:33][C:27]([CH2:28][CH2:29][PH:30](=[O:31])[OH:32])=[CH:26][C:25]=3[O:35][CH3:36])[N:14]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 178485574HCID 178485574、化合物2 回

生成物 1

HCID 178485575HCID 178485575、化合物収率 79%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

(4-{[4-{[6-bromo-2-(methylcarbamoyl)pyridin-3-yl]amino}-5-(trifluoromethyl) pyrimidin-2-yl]amino}-3-methoxybenzyl)methylphosphinate (Compound 61C, 130 mg, 0.215 mmol) in pyridine (10 mL) was charged with bromotrimethylsilane (0.171 mL, 1.29 mmol). The reaction mixture stirred at rt for 16 hrs. The reaction was concentrated in vacuo to solid to afford 100 mg of the title compound (79%). 1H NMR (400 MHz, CD3OD) δ 9.04 (br. s., 1H), 8.36 (s, 1H), 7.72 (br. s., 1H), 7.56 (d, J=8.8 Hz, 1H), 7.05 (s, 1H), 6.84-6.95 (m, 1H), 3.86 (s, 3H), 3.20 (d, J=17.7 Hz, 2H), 2.94 (s, 3H), 1.42 (s, 3H). MS (ESI): m/z=589.38/591.37 [M+H]+. UPLC: tR=1.19 min (UPLC-TOF: polar—2 min).

後処理

  1. concentrationThe reaction was concentrated in vacuo to solid

出典と根拠

ORDレコード
ord-942d2e2da3364bb4a0b3f689a91fff3a
出典データセット
uspto-grants-2015_09
特許番号
US09133224B2

反応ノート

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