Hydrochloric Acid → HCID 86595209、化合物

HRID 243519

反応式

HRID 243519 の反応式
[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028Tetrahydrofuran2 回HCID 438061,2-Diaminocyclohexane, trans-HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

生成物 1

HCID 86595209HCID 86595209、化合物収率 82.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-43534b07de5b47c4bf5d893c09df7a0a
出典データセット
uspto-grants-2014_02
特許番号
US08653259B2

関連ノート

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