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Ethanol → N-methyl-N-[4-[[(Z)-(7-oxo-6H-pyrrolo[2,3-g][1,3]benzothiazol-8-ylidene)methyl]amino]phenyl]acetamide

HRID 2415075
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HRID 2415075 반응식
CN(C)[CH:3]1[C:14]2[C:6](=[CH:7][CH:8]=[C:9]3[C:13]=2[S:12](=C)[CH:11]=[N:10]3)[NH:5][C:4]1=[O:16].[CH2:18]([OH:20])[CH3:19]>C(OCC)C>[CH3:4][N:5]([C:6]1[CH:14]=[CH:13][C:9]([NH:10]/[CH:11]=[C:3]2\[C:4](=[O:16])[NH:5][C:6]3[C:14]\2=[C:13]2[S:12][CH:11]=[N:10][C:9]2=[CH:8][CH:7]=3)=[CH:8][CH:7]=1)[C:18](=[O:20])[CH3:19]
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참가 물질

4

반응물 2

HCID 702Ethanol2회HCID 865855238-Dimethylamino-methylene-6,8-dihydro-1-thia-3,6diaza-as-indacen-7one

생성물 1

HCID 178474551N-methyl-N-[4-[[(Z)-(7-oxo-6H-pyrrolo[2,3-g][1,3]benzothiazol-8-ylidene)methyl]amino]phenyl]acetamide수율 64%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
90 °C

실험 절차

A mixture of 8-dimethylamino-methylene-6,8-dihydro-1-thia-3,6-diaza-as-indacen-7-one (Procedure E, 0.040 g, 0.163 mmol), 4-amino-N-methylacetanilide (0.040 g, 0.244 mmol) in absolute ethanol (5 ml) was heated with stirring at 90° C. for 16 h. The reaction was diluted with ethanol and diethyl ether and the product collected by filtration to yield 0.038 g (64%) of the title compound. 1H NMR (DMSO-d6): δ11.03 (d,1H, J=12.3 Hz), 10.84 (s,1H), 9.23 (s,1H), 8.02 (d,1H, J=12.3 Hz), 7.78 (d,1H, J=8.4 Hz), 7.48 (d,2H, J=8.2 Hz), 7.35 (d,2H, J=8.2 Hz), 7.09 (d,1H, J=8.4 Hz), 3.11 (s,3H), 1.76 (s, 3H); ES-MS m/z 363 (M−H).

후처리

  1. temperaturewas heated
  2. filtrationthe product collected by filtration

출처 및 근거

ORD 기록
ord-8708df8bd868479b8e753daf290ea022
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06818632B2

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