Sulfuric Acid → 4-(2-sulfanylidene-2,3-dihydro-1H-imidazol-1-yl)benzoic acid

HRID 64844

反応式

HRID 64844 の反応式
S(=O)(=O)(O)O.[C:6]([C:11]1[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][CH2:21][CH:22](OCC)OCC)=[S:19])=[CH:13][CH:12]=1)([O:8]CC)=[O:7]>O>[C:6]([C:11]1[CH:12]=[CH:13][C:14]([N:17]2[CH:22]=[CH:21][NH:20][C:18]2=[S:19])=[CH:15][CH:16]=1)([OH:8])=[O:7]

参加物

4

反応物 2

HCID 1118Sulfuric AcidHCID 4842498N-(4-carboethoxyphenyl)-N'-(2,2-diethoxyethyl)thiourea

生成物 1

HCID 137257144-(2-sulfanylidene-2,3-dihydro-1H-imidazol-1-yl)benzoic acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

400 ml of 30% sulfuric acid was added to 80 g of N-(4-carboethoxyphenyl)-N'-(2,2-diethoxyethyl)thiourea, and the mixture was refluxed for 1 hour using an oil bath. The reaction mixture was cooled to room temperature, then 600 ml of water was added thereto, followed by cooling in an ice bath. Crystals precipitated were collected by filtration, then washed successively with 200 ml of water, 100 ml of isopropyl alcohol, and 100 ml of hexane. Yield: 48 g (92.8 mol%).

後処理

  1. temperaturethe mixture was refluxed for 1 hour
  2. temperatureby cooling in an ice bath
  3. customCrystals precipitated
  4. filtrationwere collected by filtration
  5. washwashed successively with 200 ml of water, 100 ml of isopropyl alcohol, and 100 ml of hexane

出典と根拠

ORDレコード
ord-5d737fca61eb4249a08d1c23ce6f277b
出典データセット
uspto-grants-1986_09
特許番号
US04610954

関連ノート

読み込み中…