Hydrochloric Acid → Benzonitrile, 4-isothiocyanato-

HRID 236539

반응식

HRID 236539 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10040ThiophosgeneHCID 133964-Aminobenzonitrile

생성물 1

HCID 17626Benzonitrile, 4-isothiocyanato-수율 88.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-407b0f0dcdc64bb782015053e106d906
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04645678

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