Hydrochloric Acid → HCID 59649710, 화합물

HRID 2081079

반응식

HRID 2081079 반응식
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]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 59649725HCID 59649725, 화합물

생성물 1

HCID 59649710HCID 59649710, 화합물

시약·촉매·용매 2

HCID 130202-Furanpropanol, tetrahydro-용매HCID 312751,4-Dioxane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-2fe3fde0ac6d4c5c9ba4aa5954be6d82
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07932390B2

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