Hydrochloric Acid → Benzonitrile, 4-isothiocyanato-

HRID 236539

反応式

HRID 236539 の反応式
[C:1]([C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1)#[N:2].Cl.[C:11](Cl)(Cl)=[S:12]>O>[C:1]([C:3]1[CH:9]=[CH:8][C:6]([N:7]=[C:11]=[S:12])=[CH:5][CH:4]=1)#[N:2]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10040ThiophosgeneHCID 133964-Aminobenzonitrile

生成物 1

HCID 17626Benzonitrile, 4-isothiocyanato-収率 88.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 6 g (0.051 mol) of 4-cyanoaniline in 50 cm3 of N hydrochloric acid is poured drop by drop into a suspension of 6.5 g (0.056 mol) of thiophosgene in 100 cm3 of water. The reaction medium is vigorously stirred for two hours at room temperature. The precipitate formed is filtered, washed with three fractions of 10 cm3 of water, then dried in vacuo in the presence of phosphorus pentoxide. The substance is recrystallized from a mixture of hexane and carbon tetrachloride. 7.2 g of 4-cyanophenyl isothiocyanate are obtained (yield 85%) of which the melting point is 117°-118° C.

後処理

  1. customThe precipitate formed
  2. filtrationis filtered
  3. washwashed with three fractions of 10 cm3 of water
  4. dry with materialdried in vacuo in the presence of phosphorus pentoxide
  5. customThe substance is recrystallized from a mixture of hexane and carbon tetrachloride

出典と根拠

ORDレコード
ord-407b0f0dcdc64bb782015053e106d906
出典データセット
uspto-grants-1987_02
特許番号
US04645678

関連ノート

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