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5-Methyl-2-phenylsulfanyl-phenylamine → 7-methyl-N-(5-methyl-2-phenylsulfanyl-phenyl)pyrido[2,3-d]pyrimidin-4-amine

HRID 607217
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HRID 607217 반응식
[C:1]([C:3]1[C:4]([N:10]=[CH:11][N:12](C)C)=[N:5][C:6]([CH3:9])=[CH:7][CH:8]=1)#[N:2].[CH3:15][C:16]1[CH:17]=[CH:18][C:19]([S:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[C:20](N)[CH:21]=1>C(O)(=O)C>[CH3:15][C:16]1[CH:17]=[CH:18][C:19]([S:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)=[C:20]([NH:2][C:1]2[C:3]3[CH:8]=[CH:7][C:6]([CH3:9])=[N:5][C:4]=3[N:10]=[CH:11][N:12]=2)[CH:21]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 433496035-Methyl-2-phenylsulfanyl-phenylamineHCID 66808573N'-(3-Cyano-6-methyl-pyridin-2-yl)-N,N-dimethyl-formamidine

생성물 1

HCID 574018897-methyl-N-(5-methyl-2-phenylsulfanyl-phenyl)pyrido[2,3-d]pyrimidin-4-amine

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution of the product from Example 10B (90 mg, 0.517 mmol) and the product from Example 5I (122 mg, 0.569 mmol) in acetic acid (1 mL) was heated at 130° C. for 1 hour. The mixture was then allowed to cool to room temperature, the resulting solid collected and washed with methanol, then dissolved 50 mg of the material in dioxane (2 mL) and added hydrochloric acid followed by removal of the solvent under vacuum to provide the title compound as a hydrochloride salt. 1H NMR (300 MHz, DMSO-D6) δ ppm: 2.37 (s, 3H), 2.74 (s, 3H), 7.18 (m, 5H), 7.24 (m, 1H), 7.37 (m, 2H), 7.81 (d, J=8.5 Hz, 1H), 8.80 (s, 1H), 8.99 (d, J=8.5 Hz, 1H), 11.82 (bs, 1H); MS (ESI)+ m/z 359 (M+H)+.

후처리

  1. customthe resulting solid collected
  2. washwashed with methanol
  3. dissolutiondissolved 50 mg of the material in dioxane (2 mL)
  4. additionadded hydrochloric acid
  5. customfollowed by removal of the solvent under vacuum

출처 및 근거

ORD 기록
ord-84bdef5172ab4b85b9a822a37cdbf933
출처 데이터셋
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07915411B2

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