4-Toluenesulfonyl chloride → HCID 12735323, 화합물

HRID 1614009

반응식

HRID 1614009 반응식
[OH-:1].[K+].[C:3]1([CH:9]([OH:18])[CH:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[OH:11])[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[S:19](Cl)([C:22]1[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=1)(=[O:21])=[O:20]>CCOCC>[C:25]1([CH3:26])[CH:27]=[CH:28][C:22]([S:19]([O:18][CH:9]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:10]([O:11][S:19]([C:22]2[CH:28]=[CH:27][C:25]([CH3:26])=[CH:24][CH:23]=2)(=[O:20])=[O:1])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)(=[O:21])=[O:20])=[CH:23][CH:24]=1

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 14797Potassium HydroxideHCID 95447Hydrobenzoin

생성물 1

HCID 12735323HCID 12735323, 화합물수율 412.1%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Potassium hydroxide (400 mg, 7.0 mmole) was added to a solution of 1,2-diphenylethane-l,2-diol (I40 mg, 0.65 mmole) in dry ether (30 mL). TsCl (286 mg, 1.5 mmole) was added. The reaction was completed after 1 hour with stirring under N2 atmosphere at RT. A white solid was obtained. The white solid was filtered and washed with dichloromethane. The combined filtrate was concentrated, Recrystallization with methylene chloride and hexane gave the crystalline solid (1.4 g, 44.6%), mp, 110-112 (decomposed), 'H-NMR(CDCl3) δ, 2.39(s, 6H CH3), 5.61(s, 2H, CH), 6.89-7.55(m, 18H, ArH).

후처리

  1. customA white solid was obtained
  2. filtrationThe white solid was filtered
  3. washwashed with dichloromethane
  4. concentrationThe combined filtrate was concentrated
  5. customRecrystallization with methylene chloride and hexane

출처 및 근거

ORD 기록
ord-3c319cfc1762498f9802c93a6ad54e50
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194651

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