Chloroform → 2-Chloro-4,5,6,7-tetrahydro-1-benzothiophen-4-amine

HRID 1282735Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1282735
Cl.[S:2]1[CH:6]=[CH:5][C:4]2[CH:7]([NH2:11])[CH2:8][CH2:9][CH2:10][C:3]1=2.C(Cl)(Cl)[Cl:13].S(Cl)(Cl)(=O)=O.[OH-].[Na+]>O>[Cl:13][C:6]1[S:2][C:3]2[CH2:10][CH2:9][CH2:8][CH:7]([NH2:11])[C:4]=2[CH:5]=1

Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 24648Sulfuryl chlorideHCID 173886004,5,6,7-Tetrahydrobenzo[b]thiophen-4-amine hydrochloride

Produkt 1

HCID 203489752-Chloro-4,5,6,7-tetrahydro-1-benzothiophen-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A sample of 11.4 grams of 4,5,6,7-tetrahydrobenzo[b]thien-4-amine hydrochloride is stirred in 150 ml. of chloroform at about 10°C., and 6.1 ml. of sulfuryl chloride is added dropwise. The mixture is stirred for 3.5 hours at room temperature, and then about 20 ml. of 50% sodium hydroxide solution is added gradually to dissolve the suspended solid. The mixture is then poured into water and extracted with chloroform twice. The extracts are dried, evaporated to dryness, and the residue is distilled to give 7.4 grams of 2-chloro-4,5,6,7-tetrahydrobenzo[b]thien-4-amine, boiling point 94°C. to 98°C./0.5 Torr.

Aufarbeitung

  1. customat about 10°C.
  2. dissolutionto dissolve the suspended solid
  3. extractionextracted with chloroform twice
  4. customThe extracts are dried
  5. customevaporated to dryness
  6. distillationthe residue is distilled

Quellen und Nachweise

ORD-Eintrag
ord-ec281e267ede4df5b57532c2e390671f
Quelldatensatz
uspto-grants-1976_08
Patentnummer
US03972895

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