Chloroiodomethane → HCID 22035697, 화합물

HRID 489100노트

반응식

HRID 489100 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 22035697HCID 22035697, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%

후처리

  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

출처 및 근거

ORD 기록
ord-581dce77fbb54a6bb0412a45771e829f
출처 데이터셋
uspto-grants-2005_12
특허 번호
US06974802B2

반응 노트

불러오는 중…