Chloroiodomethane → HCID 22035697、化合物

HRID 489100ノート

反応式

HRID 489100 の反応式
[CH3:1][O:2][C:3]1[CH:19]=[CH:18][C:6]([CH2:7][O:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([OH:15])=[O:14])=[CH:11][CH:10]=2)=[CH:5][CH:4]=1.[OH-].C([N+](CCCC)(CCCC)CCCC)CCC.I[CH2:39][Cl:40]>O1CCOCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][O:8][C:9]2[CH:17]=[CH:16][C:12]([C:13]([O:15][CH2:39][Cl:40])=[O:14])=[CH:11][CH:10]=2)=[CH:18][CH:19]=1

参加物

5

反応物 3

HCID 11644ChloroiodomethaneHCID 2723671Tetrabutylammonium HydroxideHCID 113344014-(4-Methoxybenzyloxy) benzoic acid

生成物 1

HCID 22035697HCID 22035697、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 4-(4-methoxybenzyloxy) benzoic acid (5.16 g, 20 mmole) in 100 ml 1,4-dioxane was added a 40% solution of tetrabutylammonium hydroxide (14.27 g, 22 mmole) and the mixture was stirred 2 hours at room temperature. The mixture was evaporated under reduced pressure and co-evaporated two times with 1,4-dioxane and two times with toluene. The dried product was dissolved in 60 ml dichloromethane and iodochloromethane (35.3 g 200 mmole) was added. The solution was stirred for two days at room temperature and evaporated under reduced pressure. About 100 ml ethyl actate was added and the organic phase washed twice with water, dried with sodium sulfate and evaporated under reduced pressure. The product was isolated by silica gel column chromatography. Yield: 4.48 g=73%

後処理

  1. customThe mixture was evaporated under reduced pressure
  2. dissolutionThe dried product was dissolved in 60 ml dichloromethane
  3. stirringThe solution was stirred for two days at room temperature
  4. customevaporated under reduced pressure
  5. additionAbout 100 ml ethyl actate was added
  6. washthe organic phase washed twice with water
  7. dry with materialdried with sodium sulfate
  8. customevaporated under reduced pressure
  9. customThe product was isolated by silica gel column chromatography

出典と根拠

ORDレコード
ord-581dce77fbb54a6bb0412a45771e829f
出典データセット
uspto-grants-2005_12
特許番号
US06974802B2

反応ノート

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