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Carbon Tetrachloride → N-(Cyclohexylcarbonimidoyl)benzenamine

HRID 1649858
ノート
印刷プレビュー

反応式

HRID 1649858 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 10921546N-(Cyclohexylcarbonimidoyl)benzenamine収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-01f18543136443c6b231024d36324b2a
出典データセット
uspto-grants-1990_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04921939

反応ノート

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