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Bms-973013 → 4-(3,4-Dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-2-[4-(2-oxo-2,3-dihydro-imidazo[4,5-b]pyridin-1-yl)-piperidin-1-yl]-benzonitrile

HRID 469409
ノート
印刷プレビュー

反応式

HRID 469409 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[C:15]3[C:10](=[N:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]2=[O:16])[CH2:3][CH2:2]1.[CH3:17][N:18]1[C:22]2[C:23]([CH3:38])=[CH:24][C:25]([C:27]([C:29]3[CH:36]=[CH:35][C:32]([C:33]#[N:34])=[C:31](F)[CH:30]=3)=[O:28])=[CH:26][C:21]=2[O:20][C:19]1=[O:39]>CN(C=O)C>[CH3:17][N:18]1[C:22]2[C:23]([CH3:38])=[CH:24][C:25]([C:27]([C:29]3[CH:36]=[CH:35][C:32]([C:33]#[N:34])=[C:31]([N:1]4[CH2:2][CH2:3][CH:4]([N:7]5[C:15]6[C:10](=[N:11][CH:12]=[CH:13][CH:14]=6)[NH:9][C:8]5=[O:16])[CH2:5][CH2:6]4)[CH:30]=3)=[O:28])=[CH:26][C:21]=2[O:20][C:19]1=[O:39]
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

4

反応物 2

HCID 22293182Bms-973013HCID 581810894-(3,4-Dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-2-fluoro-benzonitrile

生成物 1

HCID 252711544-(3,4-Dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-2-[4-(2-oxo-2,3-dihydro-imidazo[4,5-b]pyridin-1-yl)-piperidin-1-yl]-benzonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
300 °C

実験手順

0.26 g (1.2 mmol) 1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-one and 93 mg (0.30 mmol) 4-(3,4-dimethyl-2-oxo-2,3-dihydro-benzoxazole-6-carbonyl)-2-fluoro-benzonitrile were combined and heated to 300° C. for approx. 10 min. Then the mixture was dissolved in DMF and purified by preparative HPLC-MS. The fractions containing the product were combined and the organic solvent was evaporated down. The residue was neutralised with 1N aqueous sodium hydroxide solution, the precipitate formed was suction filtered, washed with water and dried.

後処理

  1. custompurified by preparative HPLC-MS
  2. additionThe fractions containing the product
  3. customthe organic solvent was evaporated down
  4. customthe precipitate formed
  5. filtrationfiltered
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-20de981dacc4436c8c382f6dde0e97b0
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629137B2

反応ノート

読み込み中…

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