Acetic Anhydride → HCID 178473836、化合物

HRID 1486594ノート

反応式

HRID 1486594 の反応式
F[C:2](F)(F)[C:3]([OH:5])=O.[Cl:8][C:9]1[CH:10]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:12]=[C:13]([Cl:15])[CH:14]=1.C(=O)(O)[O-].[Na+].C(OC(=O)C)(=O)C>C(#N)C>[Cl:15][C:13]1[CH:12]=[C:11]([NH:16][C:17]2[N:21]=[C:20]([NH:22][CH:23]3[CH2:28][CH2:27][N:26]([C:3](=[O:5])[CH3:2])[CH2:25][CH2:24]3)[NH:19][N:18]=2)[CH:10]=[C:9]([Cl:8])[CH:14]=1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 178478184HCID 178478184、化合物

生成物 1

HCID 178473836HCID 178473836、化合物収率 84%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirred suspension of N3-(3,5-dichlorophenyl)-N5-(piperidin-4-yl)-1H-1,2,4-triazole-3,5-diamine 2,2,2-trifluoroacetate (50 mg, 0.113 mmol) in acetonitrile (5 mL), was added saturated sodium bicarbonate solution (5 mL) and acetic anhydride (14 mg, 0.136 mmol). The reaction mixture was stirred overnight at rt. The solution was extracted with EtOAc (3×10 mL) and dried with sodium sulfate. Removal of solvent gave the crude product, which was purified by flash chromatography to give 35 mg (84%) desired product as a white solid. MS +m/z: 369.0 (M+H)+

後処理

  1. extractionThe solution was extracted with EtOAc (3×10 mL)
  2. dry with materialdried with sodium sulfate
  3. customRemoval of solvent
  4. customgave the crude product, which
  5. customwas purified by flash chromatography

出典と根拠

ORDレコード
ord-3a2caf15307d4b4381b6663471d222b8
出典データセット
uspto-grants-2016_08
特許番号
US09428469B2

反応ノート

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