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Ammonium Acetate → HCID 13207875, 화합물

HRID 918249
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HRID 918249 반응식
[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]([C:16]1[CH:29]=[CH:28][C:27]([N+:30]([O-:32])=[O:31])=[CH:26][C:17]=1[C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)[C:10](=[O:15])C(Cl)(Cl)Cl.C([O-])(=O)C.[NH4+:37]>C(O)(C)(C)C>[CH:1]12[CH2:7][CH:4]([CH2:5][CH2:6]1)[CH2:3][CH:2]2[CH2:8][N:9]1[C:16]2[C:17](=[CH:26][C:27]([N+:30]([O-:32])=[O:31])=[CH:28][CH:29]=2)[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:37][C:10]1=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 517165Ammonium Acetate2회HCID 54358427HCID 54358427, 화합물

생성물 1

HCID 13207875HCID 13207875, 화합물

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

To a solution of 2.5 g of 2-[ N-(2-norbornylmethyl)trichloroacetamido]-5-nitrobenzophenone in 50 ml of tert-butyl alcohol was added 2 g of ammonium acetate and the resulting mixture was heated under reflux for 7 hours. Then 2 g of ammonium acetate was added thereto and the reaction was continued for additional 8 hours. The solvent was removed under reduced pressure, and the residue was extracted with chloroform. The chloroform extract was washed with water, dried over anhydrous sodium sulfate, and evaporated to dryness. The residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether to give 1-(2-norbornylmethyl)-4-phenyl-6-nitro-2(1H)-quinazolinone, m.p. 160°C.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 7 hours
  3. customThe solvent was removed under reduced pressure
  4. extractionthe residue was extracted with chloroform
  5. extractionThe chloroform extract
  6. washwas washed with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. customevaporated to dryness
  9. customThe residual oil was crystallized from a mixture of carbon tetrachloride and diethyl ether

출처 및 근거

ORD 기록
ord-8f1e1147a88e41e3ae2d089d948350a5
출처 데이터셋
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03970654

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