Hydrochloric Acid → 19430-31-0

HRID 1262831노트

반응식

HRID 1262831 반응식
[ClH:1].N[C:3]1[S:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[N:6][N:7]=1.N([O-])=O.[Na+]>O>[Cl:1][C:3]1[S:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([Cl:14])=[CH:10][CH:9]=2)=[N:6][N:7]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 6683925-(4-Chlorophenyl)-1,3,4-thiadiazol-2-amineHCID 23668193Sodium Nitrite

생성물 1

HCID 1331877519430-31-0

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
-5 °C

실험 절차

Stirred 37% hydrochloric acid, 225 ml, was cooled in a salt-ice bath, and 2-amino-5-(4-chlorophenyl)-1,3,4-thiadiazole (18.3 g, 0.087 mole) was added. The mixture was cooled to -5° C., and a solution of sodium nitrite (25.0 g, 0.338 mole) in 100 ml of water was added dropwise during a one hour period. Upon complete addition, the reaction mixture was allowed to warm to room temperature, where it was stirred for 16 hours. The reaction mixture was heated for one hour on a steam bath, cooled, then filtered to isolate the precipitated solid. The solid was recrystallized from ethanol to give 2-chloro-5-(4-chlorophenyl)-1,3,4-thiadiazole (6.0 g, mp 125°-127° C.).

후처리

  1. temperaturewas cooled in a salt-ice bath
  2. additionUpon complete addition
  3. temperatureto warm to room temperature
  4. temperatureThe reaction mixture was heated for one hour on a steam bath
  5. temperaturecooled
  6. filtrationfiltered
  7. customto isolate the precipitated solid
  8. customThe solid was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-ee467a54324c421591f0c6b8cc8780de
출처 데이터셋
uspto-grants-1984_06
특허 번호
US04454147

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