Ammonium Hydroxide → HCID 19759748、化合物

HRID 1586762ノート

反応式

HRID 1586762 の反応式
S(Cl)([Cl:3])=O.O[CH:6]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[Cl:26])[CH:7]([N:15]1[CH:19]=[CH:18][N:17]=[CH:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:14].[OH-].[NH4+]>C1C=CC=CC=1>[Cl:3][CH:6]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[Cl:26])[CH:7]([N:15]1[CH:19]=[CH:18][N:17]=[CH:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Cl:14]

参加物

5

反応物 3

HCID 14923Ammonium HydroxideHCID 24386Thionyl ChlorideHCID 13269112HCID 13269112、化合物

生成物 1

HCID 19759748HCID 19759748、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A solution of 6 g (0.05 mole) of thionyl chloride dissolved in 20 ml of benzene is added dropwise to a solution containing 11 g (0.033 mole) of 1-[2-hydroxy-1,2-di-(2-chlorophenyl)ethyl] imidazole and 150 ml of benzene at room temperature. The reaction mixture is heated to reflux for 3 hours and is then made basic with 10% ammonium hydroxide solution. The organic product is extracted with ether and the combined ether extracts are washed with water, saturated sodium chloride solution, and dried over magnesium sulfate. Solvent is evaporated to give 11 g of a brown oil. This material is further purified by converting to its hydrochloride salt and back neutralized to the free base to give 8.2 g of the expected product.

後処理

  1. additionis added dropwise to a solution
  2. temperatureThe reaction mixture is heated
  3. temperatureto reflux for 3 hours
  4. extractionThe organic product is extracted with ether
  5. washthe combined ether extracts are washed with water, saturated sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customSolvent is evaporated

出典と根拠

ORDレコード
ord-844aecbd1e3544ec8b426b3a603db480
出典データセット
uspto-grants-1993_06
特許番号
US05216007

反応ノート

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