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1,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamine → HCID 69449408, 화합물

HRID 1296726
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HRID 1296726 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:16]([C:17](=[O:19])[CH3:18])=[C:15]3[N:10]([C:11]([S:20][CH3:21])=[N:12][CH:13]=[CH:14]3)[N:9]=2)=[CH:4][CH:3]=1.C(O[CH:27](OC(C)(C)C)[N:28]([CH3:30])[CH3:29])(C)(C)C>>[CH3:27][N:28]([CH3:30])/[CH:29]=[CH:18]/[C:17]([C:16]1[C:8]([C:5]2[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=2)=[N:9][N:10]2[C:15]=1[CH:14]=[CH:13][N:12]=[C:11]2[S:20][CH3:21])=[O:19]
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참가 물질

3

반응물 2

HCID 5477121,1-bis(1,1-dimethylethoxy)-N,N,N-trimethylamineHCID 69448731HCID 69448731, 화합물

생성물 1

HCID 69449408HCID 69449408, 화합물수율 60%

반응 조건

온도
120 °C

실험 절차

To 1-[2-(4-fluorophenyl)-7-(methylsulfanyl)pyrazolo[1,5-c]pyrimidin-3-yl]ethanone (1.24 g, 4.12 mmol) was added 1,1-di-tert-butoxy-N,N-dimethylmethanamine (15 mL) and the mixture heated to 120° C. for 1 hour. The reaction was allowed to cool to room temperature and stirred for 16 hours. The mixture was diluted with hexanes. The precipitate was collected by filtration and air dried to yield (2E)-3-(dimethylamino)-1-[2-(4-fluorophenyl)-7-(methylsulfanyl)pyrazolo[1,5-c]pyrimidin-3-yl]prop-2-en-1-one (880 mg, 60%). 1H NMR (DMSO): δ 8.03 (d, 1H), 7.72–7.82 (m, 3H), 7.57 (d, 1H), 7.37 (t, 2H), 5.08 (d, 1H), 3.04 (bs, 3H), 2.71 (s, 3H), 2.52 (bs, 3H). MS m/z 357 (M+1).

후처리

  1. temperatureto cool to room temperature
  2. filtrationThe precipitate was collected by filtration and air
  3. customdried

출처 및 근거

ORD 기록
ord-3e2f0d1a1c4e4f7d9214f1174e5ff7dc
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07247626B2

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