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P-Anisidine → HCID 53345317、化合物

HRID 1464992
ノート
印刷プレビュー

反応式

HRID 1464992 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:20])[NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)=[CH:4][C:3]=1[NH:21][C:22]([C:24]1[C:28]2[N:29]=[CH:30][N:31]=[C:32](S(C)=O)[C:27]=2[S:26][CH:25]=1)=[O:23].CCN(C(C)C)C(C)C.[CH3:45][O:46][C:47]1[CH:52]=[CH:51][C:50]([NH2:53])=[CH:49][CH:48]=1>O1CCOCC1.C(OCC)(=O)C>[CH3:45][O:46][C:47]1[CH:52]=[CH:51][C:50]([NH:53][C:32]2[C:27]3[S:26][CH:25]=[C:24]([C:22]([NH:21][C:3]4[CH:4]=[C:5]([C:8](=[O:20])[NH:9][C:10]5[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:18])([F:19])[F:17])[CH:11]=5)[CH:6]=[CH:7][C:2]=4[CH3:1])=[O:23])[C:28]=3[N:29]=[CH:30][N:31]=2)=[CH:49][CH:48]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7732P-AnisidineHCID 81531DiisopropylethylamineHCID 68263099HCID 68263099、化合物

生成物 1

HCID 53345317HCID 53345317、化合物収率 81%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

N-(2-methyl-5-(3-(trifluoromethyl)phenylcarbamoyl)phenyl)-4-(methylsulfinyl)thieno[3,2-d]pyrimidine-7-carboxamide (30 mg, 0.060 mmol) was dissolved in dioxane (1 mL) and DIPEA (20 μL, 0.119 mmol) and 4-methoxybenzeneamine (37 mg, 0.298 mmol) were added thereto. The reaction mixture was stirred at 120° C. for 18 hours, cooled to room temperature, diluted with ethyl acetate and washed with a brine. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. The resulting mixture was purified by silica gel chromatography to obtain the title compound (28 mg, 81% yield).

後処理

  1. temperaturecooled to room temperature
  2. washwashed with a brine
  3. dry with materialThe organic layer was dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting mixture was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-6143811d065547b2996062ae851c79dc
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08999973B2

反応ノート

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