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Sodium Bicarbonate → HCID 18957084, 화합물

HRID 1885357
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HRID 1885357 반응식
F[B-](F)(F)F.C([O+:8]([CH2:11][CH3:12])[CH2:9][CH3:10])C.[Cl:13][C:14]1[CH:22]=C2[C:17]([CH2:18][NH:19]C2=O)=[CH:16][CH:15]=1.C(=O)([O-])O.[Na+]>C(Cl)Cl>[CH2:11]([O:8][C:9]1[C:10]2[C:17](=[CH:16][CH:15]=[C:14]([Cl:13])[CH:22]=2)[CH2:18][N:19]=1)[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 516892Sodium BicarbonateHCID 2723982Triethyloxonium tetrafluoroborateHCID 124964756-Chloro-2,3-dihydro-1H-isoindol-1-one

생성물 1

HCID 18957084HCID 18957084, 화합물수율 88.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 151 g of triethyloxonium tetrafluoroborate in 3200 ml of methylene chloride was stirred under argon at room temperature for 3.5 hours after the addition of 106.6 g of 6-chloro-2,3-dihydro-1H-isoindol-1-one. The mixture was then treated within 40 minutes with 1.28 l of saturated sodium hydrogen carbonate solution, the organic phase was separated and washed with 1.28 l of water. After drying over sodium sulphate the organic phase was filtered and evaporated. The residue was taken up in 1.3 l of diethyl ether, whereupon it was stirred at room temperature for about 30 minutes. After removing insoluble material by filtration the filtrate was evaporated. There was obtained 110.5 g of 1-ethoxy-6-chloro-3H-isoindole with a m.p. of 64°-66°.

후처리

  1. customthe organic phase was separated
  2. washwashed with 1.28 l of water
  3. dry with materialAfter drying over sodium sulphate the organic phase
  4. filtrationwas filtered
  5. customevaporated
  6. customAfter removing insoluble material
  7. filtrationby filtration the filtrate
  8. customwas evaporated

출처 및 근거

ORD 기록
ord-77472a446eb3496abc51dde50aaa3f4c
출처 데이터셋
uspto-grants-1992_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05143912

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