Hydrochloric Acid → HCID 178524450、化合物

HRID 648898

反応式

HRID 648898 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 178524450HCID 178524450、化合物収率 120.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-09ca77bdf0cc43acaceb3c71a6aa069e
出典データセット
uspto-grants-1988_04
特許番号
US04737452

関連ノート

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