Hydrochloric Acid → HCID 59406948, 화합물

HRID 80731

반응식

HRID 80731 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 59406948HCID 59406948, 화합물수율 72.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-da7ce3c1c6e449a6b35a16527eb920d4
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846676B2

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