Sodium Hydroxide → Ethyl 2,3-dihydro-2-vinyl-1H-indene-2-carboxylate

HRID 1494599

반응식

HRID 1494599 반응식
[OH-].[Na+].Br[CH2:4][C:5]1[C:6]([CH2:11]Br)=[CH:7][CH:8]=[CH:9][CH:10]=1.[C:13]([O:18][CH2:19][CH3:20])(=[O:17])[CH2:14][CH:15]=[CH2:16]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH:15]([C:14]1([C:13]([O:18][CH2:19][CH3:20])=[O:17])[CH2:11][C:6]2[C:5](=[CH:10][CH:9]=[CH:8][CH:7]=2)[CH2:4]1)=[CH2:16]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 66665o-Bis(bromomethyl)benzeneHCID 74172Ethyl vinylacetate

생성물 1

HCID 19828699Ethyl 2,3-dihydro-2-vinyl-1H-indene-2-carboxylate

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 1140Toluene용매2회

실험 절차

Tetrabutylammonium bromide (0.31 g) and 48% NaOH solution (9 ml) were added to a flask. α,α'-dibromo-o-xylene (5.0 g) in toluene (15 ml) was then added to the flask. The mixture was stirred and ethyl 3-butenoate (2.16 g) in toluene (15 ml) was added dropwise at room temperature. After the addition the temperature was slowly raised to +60° C. The mixture was stirred at this temperature for 3.5 hours and then cooled. The toluene layer was separated, washed with water and evaporated at reduced pressure to give the desired product.

후처리

  1. additionAfter the addition the temperature
  2. temperaturewas slowly raised to +60° C
  3. stirringThe mixture was stirred at this temperature for 3.5 hours
  4. temperaturecooled
  5. customThe toluene layer was separated
  6. washwashed with water
  7. customevaporated at reduced pressure

출처 및 근거

ORD 기록
ord-fcd5f311a99c451cb83ce258f6480ff3
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026868

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