Methanesulfonic Acid → HCID 178420078, 화합물

HRID 1935748노트

반응식

HRID 1935748 반응식
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

참가 물질

5

반응물 3

HCID 6395Methanesulfonic AcidHCID 14798Sodium HydroxideHCID 178479685HCID 178479685, 화합물

생성물 1

HCID 178420078HCID 178420078, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-55c9151904b94131abe3c239254677d2
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06388090B2

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