Hydrochloric Acid → 2-[(2-Aminoethyl)thiomethyl]pyrazine hydrochloride

HRID 26843

반응식

HRID 26843 반응식
[Cl:1][CH2:2][C:3]1[CH:8]=[N:7][CH:6]=[CH:5][N:4]=1.[Na].Cl.[NH2:11][CH2:12][CH2:13][SH:14].Cl>C(O)C>[ClH:1].[NH2:11][CH2:12][CH2:13][S:14][CH2:2][C:3]1[CH:8]=[N:7][CH:6]=[CH:5][N:4]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 9082Cysteamine HydrochlorideHCID 170169Pyrazine, 2-(chloromethyl)-HCID 5360545Sodium

생성물 1

HCID 205578042-[(2-Aminoethyl)thiomethyl]pyrazine hydrochloride

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Chloromethylpyrazine (6.4 g.) was added over 20 minutes to a solution freshly prepared from sodium (0.23 g.) in ethanol (50 ml.) to which cysteamine hydrochloride (5.7 g.) had been added gradually at 0° and stirred at this temperature for 2 hours. The suspension finally obtained was stirred at room temperature overnight, acidified with hydrochloric acid (pH 5) and concentrated under reduced pressure. The dry residue was extracted with ethanol and the extracts filtered and concentrated to give the crude product. Extraction with isopropyl alcohol, with the removal of some polymeric material and the addition of ether gave a cream colored solid (3.5 g.), which was recrystallised from ethanol-ether to furnish 2-[(2-aminoethyl)thiomethyl]pyrazine hydrochloride, m.p. 144°-146°.

후처리

  1. additionhad been added gradually at 0°
  2. customThe suspension finally obtained
  3. stirringwas stirred at room temperature overnight
  4. concentrationconcentrated under reduced pressure
  5. extractionThe dry residue was extracted with ethanol
  6. filtrationthe extracts filtered
  7. concentrationconcentrated
  8. customto give the crude product
  9. extractionExtraction with isopropyl alcohol
  10. customwith the removal of some polymeric material
  11. additionthe addition of ether
  12. customgave a cream colored solid (3.5 g.), which
  13. customwas recrystallised from ethanol-ether

출처 및 근거

ORD 기록
ord-0f8783500cad4e078754c0b9ea69f252
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151288

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