Sodium Hydroxide → 9-Trifluoromethoxy-6H-1,3,3a,6-tetraaza-benzo[e]azulen-5-one

HRID 2241871ノート

反応式

HRID 2241871 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][C:13]([F:16])([F:15])[F:14])=[CH:8][C:7]=1[C:17]1[NH:18][N:19]=[CH:20][N:21]=1)=[O:4].[OH-].[Na+].[Cl-].[NH4+]>O1CCOCC1>[F:14][C:13]([F:16])([F:15])[O:12][C:9]1[CH:10]=[CH:11][C:6]2[NH:5][C:3](=[O:4])[CH2:2][N:18]3[C:17](=[N:21][CH:20]=[N:19]3)[C:7]=2[CH:8]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 25517Ammonium ChlorideHCID 686936732-Chloro-N-[2-(2H-[1,2,4]triazol-3-yl)-4-trifluoromethoxy-phenyl]-acetamide

生成物 1

HCID 1363351829-Trifluoromethoxy-6H-1,3,3a,6-tetraaza-benzo[e]azulen-5-one収率 24.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 2-chloro-N-[2-(2H-[1,2,4]triazol-3-yl)-4-trifluoromethoxy-phenyl]-acetamide (3.15 g, 9.82 mmol) in dioxane (100 mL) was added aqueous sodium hydroxide (32%, 2.18 mL, 23.6 mmol) and the reaction mixture was stirred for 19 h at ambient temperature. It was poured onto aqueous ammonium chloride (1M, 50 mL) and the organic solvent was removed by destillation. The resulting suspension was filtered and the solid was washed with ice-cold water (50 mL). Drying in vacuo afforded the title compound (682 mg, 24%) as a light yellow solid. MS: m/e=285.0 [M+H]+.

後処理

  1. customthe organic solvent was removed by destillation
  2. filtrationThe resulting suspension was filtered
  3. washthe solid was washed with ice-cold water (50 mL)
  4. customDrying in vacuo

出典と根拠

ORDレコード
ord-15ef0c7686464e3cac77fadca1cd90fa
出典データセット
uspto-grants-2010_03
特許番号
US07671048B2

反応ノート

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