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Carbon Tetrachloride → N-(Cyclohexylcarbonimidoyl)benzenamine

HRID 1649858
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HRID 1649858 반응식
[CH:1]1([NH:7][C:8]([NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=S)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)Cl.C(N(CC)CC)C>C(Cl)Cl>[CH:11]1([N:10]=[C:8]=[N:7][C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1
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참가 물질

6

반응물 4

HCID 5943Carbon TetrachlorideHCID 8471TriethylamineHCID 11776TriphenylphosphineHCID 7663061-Cyclohexyl-3-phenyl-2-thiourea

생성물 1

HCID 10921546N-(Cyclohexylcarbonimidoyl)benzenamine수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

A solution containing 2.0 g (8.55 mmol) of N-cyclohexyl-N'-phenylthiourea, 2.9 g (11.1 mmol) of triphenyl phosphine and 1.16 cm3 (12 mmol) of carbon tetrachloride in 12 cm3 of methylene chloride, is treated with 1.19 cm3 (8.55 mmol) of triethylamine. The solution is heated for 2 hours, the precipitate which forms is eliminated by filtration and the filtrate is concentrated to dryness. The residue obtained is extracted with hexane and then filtered. The filtrates are then concentrated to dryness and 1.7 g (yield 100%) of the desired carbodiimide is obtained in the form of an oil.

후처리

  1. temperatureThe solution is heated for 2 hours
  2. filtrationthe precipitate which forms is eliminated by filtration
  3. concentrationthe filtrate is concentrated to dryness
  4. customThe residue obtained
  5. extractionis extracted with hexane
  6. filtrationfiltered
  7. concentrationThe filtrates are then concentrated to dryness

출처 및 근거

ORD 기록
ord-01f18543136443c6b231024d36324b2a
출처 데이터셋
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04921939

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