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Hydrochloric Acid → HCID 178479593、化合物

HRID 1262644
ノート
印刷プレビュー

反応式

HRID 1262644 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 178497688HCID 178497688、化合物

生成物 1

HCID 178479593HCID 178479593、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-79c76b8d3d1f4e08a4584caba3c58782
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04452985

反応ノート

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