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Tin atom → HCID 20027814, 화합물

HRID 1722875
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반응식

HRID 1722875 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10]23[CH2:16][CH:14]([CH2:15]2)[C:13](=[O:17])[N:12]([CH2:18][C:19]#[CH:20])[C:11]3=[O:21])=[CH:6][CH:5]=1)([O-])=O.[Sn]>O.Cl>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]([C:10]23[CH2:15][CH:14]([CH2:16]2)[C:13](=[O:17])[N:12]([CH2:18][C:19]#[CH:20])[C:11]3=[O:21])=[CH:8][CH:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 5352426Tin atomHCID 200278321-(4-Nitrophenyl)-3-propargyl-3-azabicyclo[3.1.1]heptane-2,4-dione

생성물 1

HCID 20027814HCID 20027814, 화합물

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매2회

실험 절차

A mixture of 1.6 g of 1-(4-nitrophenyl)-3-propargyl-3-azabicyclo[3.1.1]heptane-2,4-dione and 4.2 g of tin powder in 12 ml of water and 12 ml of concentrated hydrochloric acid is stirred at 100° for 1 hour. After cooling to room temperature, the reaction mixture is diluted with a little water, filtered and rendered alkaline by the addition of sodium hydroxide solution. The reaction mixture is extracted with ethyl acetate, and the organic phase is washed neutral with dilute sodium chloride solution, dried over magnesium sulphate and concentrated by evaporation. After purification by chromatography over silica gel in the system ethyl acetate/hexane 1:1, the title compound is obtained. Rf (ethyl acetate/hexane 1:1)=0.15.

후처리

  1. filtrationfiltered
  2. additionby the addition of sodium hydroxide solution
  3. extractionThe reaction mixture is extracted with ethyl acetate
  4. washthe organic phase is washed neutral with dilute sodium chloride solution
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated by evaporation
  7. customAfter purification by chromatography over silica gel in the system ethyl acetate/hexane 1:1

출처 및 근거

ORD 기록
ord-548cc18a3c584ba79c76ddc8efd544a2
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04857660

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