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3-Chloro-2-methylaniline → Friluglanstat

HRID 1505771
ノート
印刷プレビュー

反応式

HRID 1505771 の反応式
[CH3:1][O:2][CH2:3][C:4]1[NH:8][C:7]2[CH:9]=[C:10]([NH:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]([F:28])([F:27])[F:26])=[O:18])[CH:11]=[C:12]([C:13]([OH:15])=O)[C:6]=2[N:5]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[Cl:53][C:54]1[C:55]([CH3:61])=[C:56]([CH:58]=[CH:59][CH:60]=1)[NH2:57].C(=O)(O)[O-].[Na+]>CN(C=O)C.C(N(CC)CC)C>[Cl:53][C:54]1[C:55]([CH3:61])=[C:56]([NH:57][C:13]([C:12]2[C:6]3[N:5]=[C:4]([CH2:3][O:2][CH3:1])[NH:8][C:7]=3[CH:9]=[C:10]([NH:16][C:17]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25]([F:26])([F:28])[F:27])=[O:18])[CH:11]=2)=[O:15])[CH:58]=[CH:59][CH:60]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 68943-Chloro-2-methylanilineHCID 516892Sodium BicarbonateHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 90229242HCID 90229242、化合物

生成物 1

HCID 71267445Friluglanstat

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8471Triethylamine溶媒

実験手順

To a solution of 2-(methoxymethyl)-6-({[2-(trifluoromethyl)phenyl]carbonyl}amino)-1H-benzimidazole-4-carboxylic acid (153 mg) in DMF (5 mL), were added HBTU (178 mg) and triethylamine (65 μL). To the mixture was added 3-chloro-2-methylaniline (56 μL) under stirring at room temperature, and the mixture was stirred overnight. The reaction mixture was poured into saturated aqueous sodium bicarbonate, and extracted with ethyl acetate. The ethyl acetate layer was washed sequentially with water and brine, dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue was purified on silica gel column chromatography to obtain N-(3-chloro-2-methylphenyl)-2-(methoxymethyl)-6-({[2-(trifluoromethyl)phenyl]carbonyl}amino)-1H-benzimidazole-4-carboxamide (165 mg) as colorless powder.

後処理

  1. stirringthe mixture was stirred overnight
  2. extractionextracted with ethyl acetate
  3. washThe ethyl acetate layer was washed sequentially with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified on silica gel column chromatography

出典と根拠

ORDレコード
ord-b3467955550c47bf8d25d926ba6d05cd
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216968B2

反応ノート

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