Trifluoroacetic acid → HCID 67173930、化合物

HRID 41106

反応式

HRID 41106 の反応式
[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]

参加物

4

反応物 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

生成物 1

HCID 67173930HCID 67173930、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

(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.

後処理

  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

出典と根拠

ORDレコード
ord-0ca3b92738254c9b985b4ed3fbde0798
出典データセット
uspto-grants-2013_09
特許番号
US08530467B2

関連ノート

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