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Chlorotrimethylsilane → HCID 44467606, 화합물

HRID 2281419
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HRID 2281419 반응식
Cl[C:2]1[N:3]=[C:4]([N:23]2[CH2:28][CH2:27][CH:26]([CH2:29][NH:30]C(=O)OC(C)(C)C)[CH2:25][CH2:24]2)[C:5]2[C:10]([C:11]#[N:12])=[CH:9][N:8](S(C3C=CC(C)=CC=3)(=O)=O)[C:6]=2[N:7]=1.[NH2:38][C:39]1[CH:44]=[CH:43][C:42]([N:45]2[CH2:50][CH2:49][N:48]([C:51](=[O:53])[CH3:52])[CH2:47][CH2:46]2)=[CH:41][CH:40]=1.C[Si](Cl)(C)C>C(O)CCC>[C:51]([N:48]1[CH2:47][CH2:46][N:45]([C:42]2[CH:43]=[CH:44][C:39]([NH:38][C:2]3[N:3]=[C:4]([N:23]4[CH2:24][CH2:25][CH:26]([CH2:29][NH2:30])[CH2:27][CH2:28]4)[C:5]4[C:10]([C:11]#[N:12])=[CH:9][NH:8][C:6]=4[N:7]=3)=[CH:40][CH:41]=2)[CH2:50][CH2:49]1)(=[O:53])[CH3:52]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6397ChlorotrimethylsilaneHCID 7362691-[4-(4-Aminophenyl)piperazin-1-yl]ethan-1-oneHCID 57990336HCID 57990336, 화합물

생성물 1

HCID 44467606HCID 44467606, 화합물수율 16%

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
135 °C

실험 절차

A mixture of tert-butyl (1-(2-chloro-5-cyano-7-tosyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)piperidin-4-yl)methylcarbamate (180 mg, 0.330 mmol), 1-(4-(4-aminophenyl)piperazin-1-yl)ethanone (137 mg, 0.625 mmol) and TMSCl (0.300 mL, 2.37 mmol) in nBuOH (5 mL) was stirred at 135° C. for 48 h. It was then concentrated in vacuo. The residue was purified by HPLC to give the titled compound (25 mg). MS 474.5 (M+H).

후처리

  1. concentrationIt was then concentrated in vacuo
  2. customThe residue was purified by HPLC

출처 및 근거

ORD 기록
ord-482481dff0c14e33b445318ebe42546c
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09139581B2

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