Hydrochloric Acid → HCID 20528504、化合物

HRID 67088ノート

反応式

HRID 67088 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([S:8][CH2:9][C:10]#[N:11])[CH:5]=[CH:4][C:3]=1[OH:12].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:24](N)[CH2:25][NH2:26].ClC1C=CC=CC=1Cl.Cl>C(O)(C)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[C:6]([S:8][CH2:9][C:10]2[NH:26][CH2:25][CH2:24][N:11]=2)[CH:5]=[CH:4][C:3]=1[OH:12]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 72391,2-DichlorobenzeneHCID 2250301,2-Ethanediamine, 4-methylbenzenesulfonate (1:?)HCID 101303832-Chloro-4-(cyanomethylthio)-phenol

生成物 1

HCID 20528504HCID 20528504、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒2 回

実験手順

A mixture of 19.95 g of 2-chloro-4-(cyanomethylthio)-phenol, 23.3 g of ethylenediamine p-toluenesulfonate and 75 ml of 1,2-dichlorobenzene was heated at 160°-175° C. with stirring under a small flow of nitrogen for 1.5 hours. After cooling the reaction mixture, the 1,2-dichlorobenzene was decanted off. The residue was slurried in water and CH2Cl2 and then basified. The CH2Cl2 layer was separated from the mixture and an insoluble gum obtained. The gum was put in solution in isopropyl alcohol, acidified with hydrochloric acid in isopropyl alcohol and then cooled. The crude product was removed by filtering and recrystallized from isopropyl alcohol. Recrystallized 2-chloro-4-(((2-imidazolin-2-yl)methyl)thio)-phenol hydrochloride was found to have a m.p. of 181°-183° C.

後処理

  1. temperaturewas heated at 160°-175° C.
  2. temperatureAfter cooling the reaction mixture
  3. customthe 1,2-dichlorobenzene was decanted off
  4. customThe CH2Cl2 layer was separated from the mixture
  5. customan insoluble gum obtained
  6. temperaturecooled
  7. customThe crude product was removed
  8. filtrationby filtering
  9. customrecrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-290b4ebf48a242a79f6c5ae8945b2210
出典データセット
uspto-grants-1982_08
特許番号
US04344958

反応ノート

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