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Carbon Tetrachloride → HCID 178516749, 화합물

HRID 1902178
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HRID 1902178 반응식
[C:1]([O:13]C)(=O)[CH2:2][NH:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)Cl.O.[NH2:40][NH2:41]>C1COCC1.O>[C:6]1([C:4]2[NH:3][CH2:2][C:1](=[O:13])[NH:41][N:40]=2)[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 14566Methyl hippurateHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 178516749HCID 178516749, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회

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온도
50 °C

실험 절차

To 5.8 g. of methyl hippurate dissolved in 35 ml THF was added 3.9 g. of triphenylphosphine and 10.0 g. of carbon tetrachloride in 15 ml THF. The mixture was heated to about 50° C. for 6 hours and 3.0 g. of hydrazine hydrate was added. The mixture was refluxed for about 18 hours, cooled and poured into water. The solution was extracted with ethyl acetate, and the organic phase was then extracted with 1 N HCl. The acidic extract was neutralized with 6 N sodium hydroxide and the product was extracted with ethyl acetate. The organic phase was dried over anhydrous magnesium sulfate and concentrated under vacuum. The solid was recrystallized from methanol to yield about 0.200 g. of solid. Yield 4%. M.P.=212°-216° C.

후처리

  1. additionwas added 3.9 g
  2. temperatureThe mixture was refluxed for about 18 hours
  3. temperaturecooled
  4. extractionThe solution was extracted with ethyl acetate
  5. extractionthe organic phase was then extracted with 1 N HCl
  6. extractionThe acidic extract
  7. extractionthe product was extracted with ethyl acetate
  8. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  9. concentrationconcentrated under vacuum
  10. customThe solid was recrystallized from methanol
  11. customto yield about 0.200 g

출처 및 근거

ORD 기록
ord-c044782e74f04c02a92de12e53bcc028
출처 데이터셋
uspto-grants-1982_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04362550

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