Trifluoroacetic acid → HCID 57691248, 화합물

HRID 1513748노트

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HRID 1513748 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]2[CH:9]=[CH:10][C:11]3[N:12]([C:14]([CH2:17][NH:18][C:19]4[C:28]5[C:23](=[CH:24][C:25]([O:29][CH3:30])=[CH:26][N:27]=5)[N:22]=[CH:21][CH:20]=4)=[N:15][N:16]=3)[N:13]=2)[CH:5]=[CH:4][C:3]=1[CH2:31][NH:32]C(=O)OC(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl.C(#N)C.O.[OH-].[Na+]>[NH2:32][CH2:31][C:3]1[CH:4]=[CH:5][C:6]([C:8]2[CH:9]=[CH:10][C:11]3[N:12]([C:14]([CH2:17][NH:18][C:19]4[C:28]5[C:23](=[CH:24][C:25]([O:29][CH3:30])=[CH:26][N:27]=5)[N:22]=[CH:21][CH:20]=4)=[N:15][N:16]=3)[N:13]=2)=[CH:7][C:2]=1[Cl:1]

참가 물질

6

반응물 2

HCID 6422Trifluoroacetic acidHCID 67967034Tert-butyl (2-chloro-4-(3-((7-methoxy-1,5-naphthyridin-4-ylamino)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)methylcarbamate

생성물 1

HCID 57691248HCID 57691248, 화합물

시약·촉매·용매 3

HCID 14798Sodium Hydroxide촉매HCID 6344Dichloromethane용매HCID 18373917Acetonitrile--water (1/1)용매

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온도
23 °C

실험 절차

To a stirring solution of tert-butyl (2-chloro-4-(3-((7-methoxy-1,5-naphthyridin-4-ylamino)methyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)phenyl)methylcarbamate (70 mg, 128 μmol) in DCM (2 mL) was added TFA (2 mL). Reaction solution stirred for 30 min at 23° C. Solvents then removed under reduced pressure and residue purified on prep-HPLC using a water/ACN (0.1% TFA) gradient. Resulting solid was dissolved in 1:1 ACN/water (1 mL) and pH adjusted to 10 with 1M NaOH (approx 10 drops). Resulting solid collected by filtration and washed with water (5 mL). MS (ESI pos. ion) m/z: 447 (MH+). Calc'd exact mass for C22H19ClN8O: 446.

후처리

  1. customReaction solution
  2. customSolvents then removed under reduced pressure and residue
  3. custompurified
  4. customResulting solid
  5. customResulting solid
  6. filtrationcollected by filtration
  7. washwashed with water (5 mL)

출처 및 근거

ORD 기록
ord-59e4a52ba1df47a194686de1db0adc88
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217177B2

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