Hydrochloric Acid → 19430-31-0

HRID 1262831ノート

反応式

HRID 1262831 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 1331877519430-31-0

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
-5 °C

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-ee467a54324c421591f0c6b8cc8780de
出典データセット
uspto-grants-1984_06
特許番号
US04454147

反応ノート

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