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Hydrochloric Acid → 1-(2-Aminocyclohexyl)-3-(2,6-dichlorophenyl)thiourea

HRID 243519
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인쇄 미리보기

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HRID 243519 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]=[C:10]=[S:11].C1COCC1.[NH2:17][C@@H:18]1[CH2:23][CH2:22][CH2:21][CH2:20][C@H:19]1[NH2:24].Cl>O>[NH2:17][CH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH:19]1[NH:24][C:10]([NH:9][C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=1[Cl:8])=[S:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028Tetrahydrofuran2회HCID 438061,2-Diaminocyclohexane, trans-HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

생성물 1

HCID 865952091-(2-Aminocyclohexyl)-3-(2,6-dichlorophenyl)thiourea수율 82.1%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

A solution of 1,3-dichloro-2-isothiocyanatobenzene (100 mg) and abs. THF (3 ml) was added dropwise slowly over a half hour to a solution of trans-1,2-diaminocyclohexane (139.9 mg) and abs. THF (3 ml). The solution was stirred at room temperature for a further 90 minutes. The reaction mixture was subsequently added to water, acidified with hydrochloric acid and extracted once with ethyl acetate. Afterwards, the mixture was basified using potassium carbonate, and extracted three times with ethyl acetate. The combined organic phases were dried over magnesium sulfate, filtered and concentrated. 128 mg of the desired product were obtained.

후처리

  1. extractionextracted once with ethyl acetate
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic phases were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-43534b07de5b47c4bf5d893c09df7a0a
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08653259B2

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