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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
ノート
印刷プレビュー

反応式

HRID 607217 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-84bdef5172ab4b85b9a822a37cdbf933
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915411B2

反応ノート

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