Hydrochloric Acid → Methyl 2-heptyloxy-4-iodobenzoate

HRID 1171430

반응식

HRID 1171430 반응식
[OH:1][C:2]1[CH:11]=[C:10]([I:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:19](I)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25].Cl>CN(C)C=O>[CH2:19]([O:1][C:2]1[CH:11]=[C:10]([I:12])[CH:9]=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5])[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 10796Cesium carbonateHCID 202741-IodoheptaneHCID 11380407Methyl 4-iodosalicylate

생성물 1

HCID 68767792Methyl 2-heptyloxy-4-iodobenzoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of methyl 2-hydroxy-4-iodobenzoate (25 g, 90 mmol), caesium carbonate (35.2 g, 108 mmol) and n-heptyl iodide (19.2 ml, 117 mmol), in 500 ml of dimethylformamide (DMF) is stirred for 10 hours at room temperature. The solution is neutralized by addition of 2N hydrochloric acid solution. The desired product is extracted by addition of ethyl acetate. The organic phase is washed with water, dried with magnesium sulfate and concentrated using a rotary evaporator. After evaporation of the solvent, 33.84 g (100%) of the expected compound are recovered in the form of a brown oil.

후처리

  1. extractionThe desired product is extracted by addition of ethyl acetate
  2. washThe organic phase is washed with water
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated
  5. customa rotary evaporator
  6. customAfter evaporation of the solvent, 33.84 g (100%) of the expected compound
  7. customare recovered in the form of a brown oil

출처 및 근거

ORD 기록
ord-9025c5aebbdb4754af04ea06696318b4
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07829588B2

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