Methyl Salicylate → 2-Hydroxybenzoic acid 2-(2-hydroxybenzoyl)hydrazide

HRID 465156

반응식

HRID 465156 반응식
[OH2:1].[NH2:2][NH2:3].CO[C:6](=[O:14])[C:7]1[C:8](=[CH:10][CH:11]=[CH:12][CH:13]=1)[OH:9].[OH2:15].CO>CO>[C:6]([NH:2][NH:3][C:6](=[O:14])[C:7]1[C:8](=[CH:10][CH:11]=[CH:12][CH:13]=1)[OH:9])(=[O:15])[C:7]1[C:13](=[CH:12][CH:11]=[CH:10][CH:8]=1)[OH:1]

참가 물질

5

반응물 3

HCID 4133Methyl SalicylateHCID 24654Hydrazine hydrate (1:1)HCID 22242641Methanol--water (1/1)

생성물 1

HCID 653032-Hydroxybenzoic acid 2-(2-hydroxybenzoyl)hydrazide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

0.5 kg (10 mol) hydrazine hydrate was heated with 3.040 kg (20 mol) salicylic acid methyl ester and 2.714 kg vaseline in a protective gas such as nitrogen or argon in the apparatus according to the invention. The water-methanol mixture produced was continuously distilled-off from the reaction mixture. After about three hours, the reaction temperature had risen to 120° C. and approximately half of the quantity of methanol expected theoretically and the entire amount of water were distilled off (0.5 kg). The hydrazide was present in the vaseline as a crystal product in paste. The heating was continued after 30 g boron trioxide was added and the temperature was kept at 150° C. The remaining methanol (0.320 kg) was distilled off. After about three hours, the reaction was complete as determined by the amount of methanol distilled off.

후처리

  1. customhad risen to 120° C.
  2. distillationthe entire amount of water were distilled off (0.5 kg)
  3. additionwas added
  4. customwas kept at 150° C
  5. distillationThe remaining methanol (0.320 kg) was distilled off
  6. waitAfter about three hours
  7. distillationdistilled off

출처 및 근거

ORD 기록
ord-fa763f0050c54319865f6bc7d5d33c9a
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550204

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