Methanesulfonic Acid → HCID 178420078、化合物

HRID 1935748ノート

反応式

HRID 1935748 の反応式
Cl.[NH:2]1[CH:6]=[C:5]([CH:7](O)[CH2:8][CH2:9][CH:10]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:4]=[CH:3]1.CS(O)(=O)=O.[OH-].[Na+]>O>[C:11]1([CH:10]2[C:17]3[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:7]([C:5]3[N:4]=[CH:3][NH:2][CH:6]=3)[CH2:8][CH2:9]2)[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 3

HCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 178479685HCID 178479685、化合物

生成物 1

HCID 178420078HCID 178420078、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of 1-(1H-imidazol-4-yl)-4,4-diphenylbutan-1-ol hydrochloride (2.0 g) and methanesulfonic acid (40 ml) was heated at 100° C. for 40 minutes. The cooled reaction mixture was poured into water and was made alkaline with sodium hydroxide solution. The product was extracted into ethyl acetate, which was washed with water, dried with sodium sulfate and evaporated under reduced pressure to give a crude product of racemic cis and trans diastereomers. The product was purified by flash chromatography (elution with a dichloromethane—methanol gradient). The base product was dissolved in ethyl acetate and converted to its hydrochloride salt with hydrogen chloride gas.

後処理

  1. customThe cooled reaction mixture
  2. extractionThe product was extracted into ethyl acetate, which
  3. washwas washed with water
  4. dry with materialdried with sodium sulfate
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-55c9151904b94131abe3c239254677d2
出典データセット
uspto-grants-2002_05
特許番号
US06388090B2

反応ノート

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