Hydrochloric Acid → Methyl 2-heptyloxy-4-iodobenzoate

HRID 1171430

反応式

HRID 1171430 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 68767792Methyl 2-heptyloxy-4-iodobenzoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9025c5aebbdb4754af04ea06696318b4
出典データセット
uspto-grants-2010_11
特許番号
US07829588B2

関連ノート

読み込み中…