Bromotrimethylsilane → HCID 178485575, 화합물

HRID 2279887노트

반응식

HRID 2279887 반응식
[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

참가 물질

4

반응물 2

HCID 76113BromotrimethylsilaneHCID 178485574HCID 178485574, 화합물2회

생성물 1

HCID 178485575HCID 178485575, 화합물수율 79%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

(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).

후처리

  1. concentrationThe reaction was concentrated in vacuo to solid

출처 및 근거

ORD 기록
ord-942d2e2da3364bb4a0b3f689a91fff3a
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133224B2

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