Hydrochloric Acid → Methyl 2-heptyloxy-4-iodobenzoate

HRID 1171436

反応式

HRID 1171436 の反応式
C(=O)([O-])[O-].[Cs+].[Cs+].[I:7][C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[C:10]([OH:18])[CH:9]=1.I[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26].Cl>CN(C=O)C>[CH2:20]([O:18][C:10]1[CH:9]=[C:8]([I:7])[CH:17]=[CH:16][C:11]=1[C:12]([O:14][CH3:15])=[O:13])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH3:26]

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収率 100%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A suspension of caesium carbonate (35.2 g, 108 mmol), methyl 4-iodo-2-hydroxybenzoate (25 g, 90 mmol), iodoheptane (19.2 ml, 117 mmol) in DMF (500 ml) is stirred for 10 hours at room temperature. The organic phase is acidified at room temperature with a 2N hydrochloric acid solution to pH 5. 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 remainder of the iodoheptane by placing the oil obtained under vacuum produced by a rotary vane pump, 33.8 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 remainder of the iodoheptane
  7. customobtained under vacuum

出典と根拠

ORDレコード
ord-0e218b050248476fb30901644d11cf9b
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…