Iodine → HCID 20467612, 화합물

HRID 1413828

반응식

HRID 1413828 반응식
[Mg].II.Br[C:5]1[CH:10]=[CH:9][C:8]([C:11]2([CH3:16])[O:15][CH2:14][CH2:13][O:12]2)=[CH:7][CH:6]=1.[CH2:17](Br)[CH:18]=[C:19]([CH3:21])[CH3:20].[Cl-].[NH4+]>O1CCCC1.O.BrCCBr>[CH3:16][C:11]1([C:8]2[CH:9]=[CH:10][C:5]([CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])=[CH:6][CH:7]=2)[O:15][CH2:14][CH2:13][O:12]1

참가 물질

9

반응물 5

HCID 807IodineHCID 25517Ammonium ChlorideHCID 700922-Butene, 1-bromo-3-methyl-HCID 6149202-(4-Bromophenyl)-2-methyl-1,3-dioxolaneHCID 5462224Magnesium

생성물 1

HCID 20467612HCID 20467612, 화합물수율 77.7%

시약·촉매·용매 3

HCID 78391,2-Dibromoethane촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매3회

실험 절차

To a mixture of 10.2 g of magnesium turnigns, 300 ml of tetrahydrofuran and a few pieces of iodine, was added 3.8 g of 1,2-dibromoethane with stirring under a stream of nitrogen. Additionally, a solution of 93.0 g of 2-(p-bromophenyl)-2-methyl-1,3-dioxolane dissolved in 300 ml of tetrahydrofuran was dropped while keeping the temperature at 50°-55° C. After dropping, the reaction mixture was stirred for 30 minutes, and cooled to room temperature. A solution of 66.0 g of prenyl bromide in 100 ml of tetrahydrofuran was then dropped to the reaction mixture while keeping the reaction temperature at 50°-55° C., which was allowed to stand for overnight at room temperature. A solution of 20 g of ammonium chloride in 50 ml of water was added. The organic layer was decanted, concentrated and dissolved in ethyl ether. The ethereal solution was washed with water, dried, concentrated and distilled to give 69.1 g of 2-methyl-2-(p-prenylphenyl)-1,3-dioxolane, b.p. 106-107 °C/0.10 mmHg.

후처리

  1. additionwas dropped
  2. customat 50°-55° C
  3. stirringthe reaction mixture was stirred for 30 minutes
  4. customat 50°-55° C.
  5. customThe organic layer was decanted
  6. concentrationconcentrated
  7. dissolutiondissolved in ethyl ether
  8. washThe ethereal solution was washed with water
  9. customdried
  10. concentrationconcentrated
  11. distillationdistilled

출처 및 근거

ORD 기록
ord-175386732090443583e4b034005d4669
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04251543

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