Trifluoroacetic acid → HCID 67173930, 화합물

HRID 41106

반응식

HRID 41106 반응식
[F:1][C:2]1[CH:7]=[C:6]([C:8](=[O:11])[NH:9][CH3:10])[CH:5]=[C:4]([F:12])[C:3]=1[C:13]1[N:17]([CH2:18][C@H:19]2[O:24][CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20]2)[C:16]2[CH:32]=[CH:33][C:34]([CH3:36])=[CH:35][C:15]=2[N:14]=1.[C:37]([OH:43])([C:39]([F:42])([F:41])[F:40])=[O:38]>C(Cl)Cl>[F:40][C:39]([F:42])([F:41])[C:37]([OH:43])=[O:38].[F:12][C:4]1[CH:5]=[C:6]([CH:7]=[C:2]([F:1])[C:3]=1[C:13]1[N:17]([CH2:18][C@H:19]2[O:24][CH2:23][CH2:22][NH:21][CH2:20]2)[C:16]2[CH:32]=[CH:33][C:34]([CH3:36])=[CH:35][C:15]=2[N:14]=1)[C:8]([NH:9][CH3:10])=[O:11]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67173392(R)-tert-butyl 2-((2-(2,6-difluoro-4-(methylcarbamoyl)phenyl)-5-methyl-1H-benzo[d]imidazol-1-yl)methyl)morpholine-4-carboxylate

생성물 1

HCID 67173930HCID 67173930, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

(R)-tert-butyl 2-((2-(2,6-difluoro-4-(methylcarbamoyl)phenyl)-5-methyl-1H-benzo[d]imidazol-1-yl)methyl)morpholine-4-carboxylate (770 mg, 1.54 mmol) was dissolved in DCM (10.0 mL). Afterward, TFA (2.00 mL) was added to the mixture at 0° C. The resulting mixture was stirred at room temperature for 1 hr and then concentrated under reduced pressure. The crude (S)-3,5-difluoro-N-methyl-4-(5-methyl-1-(morpholin-2-ylmethyl)-1H-benzo[d]imidazol-2-yl)benzamide trifluoroacetic acid salt product was used without further purification (790 mg) in the next step. It was analyzed on analytical HPLC MS using the high pH gradient method (mobile phase: 5-95% B; A: H2O with 10 mM NH4CO3 and 0.375% NH4OH v/v; B: CH3CN; 2.25 min run; X-Bridge C18; column size: 2.1×30 mm; particle size: 5 μm). MS m/z 401.3 [M+H]+ (ESI), Rt 1.37 min.

후처리

  1. concentrationconcentrated under reduced pressure
  2. customThe crude (S)-3,5-difluoro-N-methyl-4-(5-methyl-1-(morpholin-2-ylmethyl)-1H-benzo[d]imidazol-2-yl)benzamide trifluoroacetic acid salt product was used without further purification (790 mg) in the next step
  3. custom2.25 min

출처 및 근거

ORD 기록
ord-0ca3b92738254c9b985b4ed3fbde0798
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08530467B2

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