Ammonium Chloride → HCID 69733599, 화합물

HRID 1062503노트

반응식

HRID 1062503 반응식
Br[CH2:2][CH:3]1[CH2:8][CH:7]2[CH2:9][CH:4]1[CH:5]=[CH:6]2.[CH2:10]([O:12][CH:13](OCC)[CH:14]=[CH2:15])[CH3:11].[Cl-].[NH4+]>O1CCCC1.[Cu]Br>[CH2:10]([O:12][CH:13]=[CH:14][CH2:15][CH2:2][CH:3]1[CH2:8][CH:7]2[CH2:9][CH:4]1[CH:5]=[CH:6]2)[CH3:11]

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 624773,3-Diethoxy-1-propeneHCID 27760625-(bromomethyl)bicyclo[2.2.1]hept-2-ene

생성물 1

HCID 69733599HCID 69733599, 화합물

시약·촉매·용매 2

HCID 24593copper(I) bromide촉매HCID 8028Tetrahydrofuran용매2회

실험 절차

A Grignard reagent was customarily prepared from 200 g of 5-bromomethyl-2-norbornene in 500 ml of dry tetrahydrofuran. The Grignard reagent was added dropwise over one hour to a mixture of 130 g of 3,3-diethoxy-1-propene, 1.0 g of copper (I) bromide and 300 ml of dry tetrahydrofuran at 20° C. Stirring was continued for 20 hours whereupon the reaction solution was added to a saturated aqueous solution of ammonium chloride to stop reaction. After hexane extraction, the organic layer was successively washed with water, saturated sodium bicarbonate water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum, yielding 5-(4-ethoxy-3-buten-1-yl)-2-norbornene.

후처리

  1. customreaction
  2. extractionAfter hexane extraction
  3. washthe organic layer was successively washed with water, saturated sodium bicarbonate water and saturated sodium chloride water
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuum

출처 및 근거

ORD 기록
ord-7bc15910770f4791a81eee156b66be35
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06962767B2

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