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Trifluoroacetic acid → HCID 66713692、化合物

HRID 1797923
ノート
印刷プレビュー

反応式

HRID 1797923 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:10]=[CH:11][C:12]3[O:16][C:15](=[O:17])[NH:14][C:13]=3[CH:18]=2)[C:5]([CH3:19])=[CH:4][N:3]=1.Cl.[F:21][C:22]1[C:27]([CH3:28])=[CH:26][C:25]([NH2:29])=[CH:24][C:23]=1[O:30][CH3:31].[C:32]([OH:38])([C:34]([F:37])([F:36])[F:35])=[O:33].ClC1N=CC=CN=1>CC(O)C>[F:35][C:34]([F:37])([F:36])[C:32]([OH:38])=[O:33].[F:21][C:22]1[C:27]([CH3:28])=[CH:26][C:25]([NH:29][C:2]2[N:7]=[C:6]([NH:8][C:9]3[CH:10]=[CH:11][C:12]4[O:16][C:15](=[O:17])[NH:14][C:13]=4[CH:18]=3)[C:5]([CH3:19])=[CH:4][N:3]=2)=[CH:24][C:23]=1[O:30][CH3:31]
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 4

HCID 6422Trifluoroacetic acidHCID 744042-ChloropyrimidineHCID 580713875-(2-Chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-oneHCID 667135964-Fluoro-3-methoxy-5-methylanilline hydrochloride

生成物 1

HCID 66713692HCID 66713692、化合物

試薬・触媒・溶媒 1

HCID 3776
Isopropanol
溶媒

反応条件

温度
77.5 °C

実験手順

Into a three-neck round-bottom flask, 5-(2-chloro-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one (33.2 g, 120 mmol) and 4-fluoro-3-methoxy-5-methylbenzenamine hydrochloride (32.19 g, 168 mmol) were added, followed by i-PrOH (750 mL) and TFA (23.1 mL, 300 mmol). The reaction mixture was stirred under nitrogen atmosphere with gentle refluxing (note: with overhead stirrer at internal temperature of 75-80° C.). After 22 h, by LC-MS, the reaction was >95% complete (note: when ≦3% of the 2-chloropyrimidine starting material remained, the reaction did not progress much further even after another day or two). The reaction mixture was cooled to room temperature, precipitate was collected by filtration, washing with i-PrOH (˜50 mL×2). Compound 5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one trifluoroacetate was obtained as a light tan color solid (still a little bit damp) and was added to a NaHCO3 aqueous solution (15.12 g (180 mmol) of NaHCO3 dissolved in 1 L of H2O). The aqueous suspension was stirred at rt overnight. Solid was collected by filtration, washing with H2O (˜150 mL×3), and was further dried under high vacuum. Free base compound 5-(2-(4-fluoro-3-methoxy-5-methylphenylamino)-5-methylpyrimidin-4-ylamino)benzo[d]oxazol-2(3H)-one was obtained as an off-white solid: 44.51 g (93.8% yield).

後処理

  1. waitthe reaction did not progress much further even after another day
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationprecipitate was collected by filtration
  4. washwashing with i-PrOH (˜50 mL×2)

出典と根拠

ORDレコード
ord-f599a7c342544afcad6195c6901b112a
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08343954B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート