p-Fluoronitrobenzene → HCID 14933055, 화합물

HRID 1030278

반응식

HRID 1030278 반응식
CC([O-])(C)C.[K+].F[C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1.[Cl:17][CH2:18][CH2:19][CH2:20][SH:21]>CS(C)=O.O>[Cl:17][CH2:18][CH2:19][CH2:20][S:21][C:8]1[CH:13]=[CH:12][C:11]([N+:14]([O-:16])=[O:15])=[CH:10][CH:9]=1

참가 물질

6

반응물 3

HCID 9590p-FluoronitrobenzeneHCID 871343-ChloropropanethiolHCID 23665647Potassium tert-butoxide

생성물 1

HCID 14933055HCID 14933055, 화합물수율 34%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매2회HCID 962Water용매

반응 조건

온도
10 °C

실험 절차

To a cooled (10° C.), stirred suspension of KOtBu (8.9 g, 0.080 mol) in DMSO (40 mL) was added a solution of 4-fluoronitrobenzene (11.2 g, 0.080 mol) and 3-chloropropanethiol (8.8 g, 0.080 mol) in DMSO (40 mL) over 10 minutes. The mixture was stirred at room temperature for 3.5 hours, diluted with water (1000 ml), and extracted with ether. The extracts were washed with brine, dried (MgSO4), and concentrated. Purification by flash chromatography (10% EtOAc/hexane) gave 6.2 g (34%) of product as a yellow solid m.p. 45°-48° C.

후처리

  1. stirringThe mixture was stirred at room temperature for 3.5 hours
  2. extractionextracted with ether
  3. washThe extracts were washed with brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customPurification by flash chromatography (10% EtOAc/hexane)

출처 및 근거

ORD 기록
ord-7e3d4cb3d6324a3a900fd6ef81d27707
출처 데이터셋
uspto-grants-1992_04
특허 번호
US05104892

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