Hydrochloric Acid → HCID 86595209, 화합물

HRID 243519

반응식

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 물질

6

반응물 4

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

생성물 1

HCID 86595209HCID 86595209, 화합물수율 82.1%

시약·촉매·용매 1

HCID 962Water용매

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
특허 번호
US08653259B2

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