Hydrochloric Acid → HCID 59406948、化合物

HRID 80731

反応式

HRID 80731 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]2[N:12]3[N:13]=[C:14]([N:17]4[CH2:21][CH:20]5[CH2:22][N:23](C(OC(C)(C)C)=O)[CH2:24][CH:19]5[CH2:18]4)[CH:15]=[CH:16][C:11]3=[N:10][C:9]=2[C:32]2[CH:37]=[CH:36][C:35]([Cl:38])=[CH:34][CH:33]=2)[CH:5]=[CH:4][N:3]=1.Cl>ClCCl>[Cl:38][C:35]1[CH:36]=[CH:37][C:32]([C:9]2[N:10]=[C:11]3[CH:16]=[CH:15][C:14]([N:17]4[CH2:21][CH:20]5[CH:19]([CH2:24][NH:23][CH2:22]5)[CH2:18]4)=[N:13][N:12]3[C:8]=2[C:6]2[CH:5]=[CH:4][N:3]=[C:2]([NH2:1])[CH:7]=2)=[CH:33][CH:34]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 59406953tert-Butyl 5-[3-(2-aminopyrid-4-yl)-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-6-yl]hexahydropyrrolo[3,4-c]pyrrole-2-carboxylate

生成物 1

HCID 59406948HCID 59406948、化合物収率 72.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.16 g (0.29 mmol) of tert-butyl 5-[3-(2-aminopyrid-4-yl)-2-(4-chlorophenyl)imidazo[1,2-b]pyridazin-6-yl]hexahydropyrrolo[3,4-c]pyrrole-2-carboxylate in 3 mL of dichloromethane are added 1.5 mL (18 mmol) of concentrated hydrochloric acid. After stirring for 1 hour at room temperature, the solvent is evaporated off under reduced pressure, the oily residue is taken up with aqueous ammonia and the product is extracted with dichloromethane. The organic phase is filtered on a hydrophobic cartridge and concentrated under reduced pressure. The solid obtained is triturated with diisopropyl ether to give 0.091 g of solid after filtering off and drying under reduced pressure.

後処理

  1. customthe solvent is evaporated off under reduced pressure
  2. extractionthe product is extracted with dichloromethane
  3. filtrationThe organic phase is filtered on a hydrophobic cartridge
  4. concentrationconcentrated under reduced pressure
  5. customThe solid obtained
  6. customis triturated with diisopropyl ether

出典と根拠

ORDレコード
ord-da7ce3c1c6e449a6b35a16527eb920d4
出典データセット
uspto-grants-2014_09
特許番号
US08846676B2

関連ノート

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