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Hydrochloric Acid → HCID 178479593, 화합물

HRID 1262644
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HRID 1262644 반응식
[NH2:1][NH2:2].C[O:4][C:5](=O)[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([C:12]2[N:13]=[C:14]([NH:17][CH:18]=[N:19][NH2:20])[S:15][CH:16]=2)[CH:7]=1.[ClH:22]>C(O)C>[ClH:22].[NH2:20][N:19]=[CH:18][NH:17][C:14]1[S:15][CH:16]=[C:12]([C:8]2[CH:7]=[C:6]([CH:11]=[CH:10][CH:9]=2)[C:5]([NH:1][NH2:2])=[O:4])[N:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 178497688HCID 178497688, 화합물

생성물 1

HCID 178479593HCID 178479593, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 10 ml. of 95% hydrazine is added 3-[2-[(aminoiminomethyl)amino]-4-thiazolyl]benzoic acid methyl ester (1.1 g., 0.004 mole). This is stirred for 1 hour at room temperature. The product precipitates out and is filtered off and rinsed with ethanol. The filtrate is reduced to dryness and ethanol is added to the residue, and the insoluble material is filtered off and combined with previously filtered solid to give a crude yield of about 1 g. of the carboxhydrazide. This crude solid is added to 40 ml. ethanol and to this is added 10 ml. of ethanolic HCl solution and the mixture is heated briefly at reflux temperature. The suspension that forms is filtered off and recrystallized from 90% aqueous ethanol to give 0.65 g. of the desired product, m.p. 275° C. (dec.).

후처리

  1. customThe product precipitates out
  2. filtrationis filtered off
  3. washrinsed with ethanol
  4. additionis added to the residue
  5. filtrationthe insoluble material is filtered off
  6. customto give a crude yield of about 1 g
  7. additionThis crude solid is added to 40 ml
  8. temperatureat reflux temperature
  9. filtrationThe suspension that forms is filtered off
  10. customrecrystallized from 90% aqueous ethanol
  11. customto give 0.65 g

출처 및 근거

ORD 기록
ord-79c76b8d3d1f4e08a4584caba3c58782
출처 데이터셋
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04452985

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