Hydrochloric Acid → HCID 59649710、化合物

HRID 2081079ノート

反応式

HRID 2081079 の反応式
COC[O:4][C:5]1[CH:6]=[C:7]([C:12]2[N:13]=[N:14][N:15]([CH3:17])[CH:16]=2)[CH:8]=[CH:9][C:10]=1[CH3:11].Cl>O1CCCC1CCCO.O1CCOCC1>[CH3:11][C:10]1[CH:9]=[CH:8][C:7]([C:12]2[N:13]=[N:14][N:15]([CH3:17])[CH:16]=2)=[CH:6][C:5]=1[OH:4]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 59649725HCID 59649725、化合物

生成物 1

HCID 59649710HCID 59649710、化合物

試薬・触媒・溶媒 2

HCID 130202-Furanpropanol, tetrahydro-溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 4-(3-methoxymethoxy-4-methyl-phenyl)-1-methyl-1H-[1,2,3]triazol (0.57 g, 2.44 mmol) (from Example 20 supra) in tetrahydrofuran-2-propanol (1:1, 20 mL) was added HCl in dioxane (4 M, 8 mL) (Aldrich). The reaction mixture was stirred at room temperature for 2 days. The solution was concentrated. The residue was diluted with ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and brine, dried (MgSO4) and concentrated. The residue was recrystallized from ethyl acetate-hexanes and dried to give 2-methyl-5-(1-methyl-1H-[1,2,3]triazol-4-yl)-phenol. (Yield 0.24 g, 52%).

後処理

  1. concentrationThe solution was concentrated
  2. additionThe residue was diluted with ethyl acetate
  3. washwashed with saturated aqueous sodium bicarbonate solution and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customThe residue was recrystallized from ethyl acetate-hexanes
  7. customdried

出典と根拠

ORDレコード
ord-2fe3fde0ac6d4c5c9ba4aa5954be6d82
出典データセット
uspto-grants-2011_04
特許番号
US07932390B2

反応ノート

読み込み中…