Potassium Hydroxide → HCID 18182294, 화합물

HRID 1359266

반응식

HRID 1359266 반응식
[Br:1]Br.[Br-].[K+].[CH2:5]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[N:13]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[OH-].[K+].S([O-])([O-])=O.[Na+].[Na+]>[Cl-].[NH4+].[NH4+].[NH4+].[NH4+].[Cl-].[Cl-].[Cl-].O>[CH2:5]([CH:12]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[N:13]1[Br:1])[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

참가 물질

8

반응물 5

HCID 14797Potassium HydroxideHCID 24408BromineHCID 24437Sodium SulfiteHCID 253877Potassium Bromide2회HCID 219422742-Benzyl-6-methoxypyridine

생성물 1

HCID 18182294HCID 18182294, 화합물

시약·촉매·용매 2

HCID 22266888HCID 22266888, 화합물촉매HCID 962Water용매2회

실험 절차

A mixed solution of 17 ml of bromine, 90 g of potassium bromide and 450 ml of water was added dropwise into a mixture of 60 g of 2-benzyl-6-methoxypyridine (Production Example 2-b), 90 g of potassium bromide, 450 ml of water, 20 g of potassium hydroxide and 2.5 g of tetraammonium chloride over 2 hours under stirring in an ice bath. After stirring overnight as it was, sodium sulfite was added thereto and the mixture was extracted with hexane. The organic phase was washed with water and brine, dried over anhydrous magnesium sulfate and the solvent was removed. The residue was subjected to silica gel column chromatography to elute with 0.5-1.5% of ethyl acetate/hexane, to give 72.5 g of the target compound.

후처리

  1. stirringAfter stirring overnight as it
  2. extractionthe mixture was extracted with hexane
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customthe solvent was removed
  6. washto elute with 0.5-1.5% of ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-0314bc1e8d6b4fe0a3167db30808daec
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06599917B1

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