Diisopropylethylamine → HCID 58386449、化合物

HRID 74628

反応式

HRID 74628 の反応式
Cl.Cl.[NH:3]1[CH2:8][CH2:7][CH:6]([N:9]2[C:17]3[C:12](=[N:13][CH:14]=[CH:15][CH:16]=3)[NH:11][C:10]2=[O:18])[CH2:5][CH2:4]1.Cl[C:20]1[N:25]=[CH:24][N:23]=[C:22]([C:26]([N:28]2[CH:36]3[CH:31]([CH2:32][CH2:33][CH2:34][CH2:35]3)[CH2:30][CH2:29]2)=[O:27])[CH:21]=1.CCN(C(C)C)C(C)C>CN(C=O)C>[N:28]1([C:26]([C:22]2[N:23]=[CH:24][N:25]=[C:20]([N:3]3[CH2:4][CH2:5][CH:6]([N:9]4[C:17]5[C:12](=[N:13][CH:14]=[CH:15][CH:16]=5)[NH:11][C:10]4=[O:18])[CH2:7][CH2:8]3)[CH:21]=2)=[O:27])[CH:36]2[CH:31]([CH2:32][CH2:33][CH2:34][CH2:35]2)[CH2:30][CH2:29]1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 222931811-(piperidin-4-yl)-1H,2H,3H-imidazo[4,5-b]pyridin-2-one dihydrochlorideHCID 58386728(6-Chloropyrimidin-4-yl)-(octahydroindol-1-yl)-methanone

生成物 1

HCID 58386449HCID 58386449、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

201 mg (0.69 mmol) 1-piperidin-4-yl-1,3-dihydroimidazo[4,5-b]pyridin-2-on-dihydrochloride were added to 184 mg (0.69 mmol) (6-chloropyrimidin-4-yl)-(octahydroindol-1-yl)-methanone and 488 μL (2.8 mmol) DIPEA in 3 mL DMF. The reaction mixture was stirred at RT over the weekend and then purified by preparative HPLC-MS. The product fractions were combined and the organic solvent was removed using the rotary evaporator. The aqueous solution was neutralised with aqueous 1N NaOH solution and the precipitate obtained was suction filtered. The precipitate was washed with water and dried.

後処理

  1. custompurified by preparative HPLC-MS
  2. customthe organic solvent was removed
  3. customthe rotary evaporator
  4. customthe precipitate obtained
  5. filtrationfiltered
  6. washThe precipitate was washed with water
  7. customdried

出典と根拠

ORDレコード
ord-854e70004035492c9ccfd59f599267b1
出典データセット
uspto-grants-2014_09
特許番号
US08829006B2

関連ノート

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