Hydrochloric Acid → HCID 178524450, 화합물

HRID 648898

반응식

HRID 648898 반응식
[N:1]([C:4]1[CH:14]=[CH:13][C:7]([C:8]([O:10]CC)=[O:9])=[CH:6][CH:5]=1)=[C:2]=[S:3].[N-:15]=[N+:16]=[N-:17].[Na+].Cl>O>[C:8]([C:7]1[CH:13]=[CH:14][C:4]([N:1]2[C:2]([SH:3])=[N:17][N:16]=[N:15]2)=[CH:5][CH:6]=1)([OH:10])=[O:9]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 71003Ethyl 4-isothiocyanatobenzoate

생성물 1

HCID 178524450HCID 178524450, 화합물수율 120.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Then, 31 g of ethyl p-isothiocyanatobenzoate and 11.7 g of sodium azide were dispersed in 300 ml of water and the dispersion was refluxed for 5 hours. The reaction mixture was cooled to room temperature and acidified (pH about 2) by the addition of concentrated hydrochloric acid. Crystals of 1-(4-ethoxycarbonylphenyl)-5-mercaptotetrazole thus deposited were collected by filtration and after adding thereto 25 g of sodium hydroxide and 500 ml of water, the mixture was stirred for 30 minutes at 70° C. The reaction mixture was cooled to room temperature, neutralized by the addition of concentrated hydrochloric acid, and crystals thus deposited were collected by filtration and recrystallized from methanol to provide 40 g of 1-(4-carboxyphenyl)-5-mercaptotetrazole. The yield was 48% and the melting point was 198° C.

후처리

  1. temperaturethe dispersion was refluxed for 5 hours
  2. filtrationCrystals of 1-(4-ethoxycarbonylphenyl)-5-mercaptotetrazole thus deposited were collected by filtration
  3. additionafter adding
  4. temperatureThe reaction mixture was cooled to room temperature
  5. additionneutralized by the addition of concentrated hydrochloric acid, and crystals
  6. filtrationthus deposited were collected by filtration
  7. customrecrystallized from methanol

출처 및 근거

ORD 기록
ord-09ca77bdf0cc43acaceb3c71a6aa069e
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04737452

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