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HCID 23053853, 화합물 → HCID 23053856, 화합물

HRID 1650196
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HRID 1650196 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:20]([NH2:22])=O)[CH:5]=[C:6]([Cl:19])[C:7]=1[S:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1>O1CCCC1>[Cl:19][C:6]1[CH:5]=[C:4]([CH:3]=[C:2]([Cl:1])[C:7]=1[S:8][C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]=[CH:11][CH:10]=1)[CH2:20][NH2:22]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 23053853HCID 23053853, 화합물

생성물 1

HCID 23053856HCID 23053856, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 25 g of 3,5-dichloro-4-[(l-naphthyl)thio]benzene carboxamide in 150 ml of dry tetrahydrofuran (THF) is treated with 230 ml of 1.0 M BH3 -THF complex. The resulting solution is heated at reflux for 16 hours. The reaction mixture is cooled with ice and quenched with excess 2 N HCl. The mixture is then made basic with NaOH and extracted with methylene chloride. The combined extracts are washed with water and dried with anhydrous magnesium sulfate. Concentration under reduced pressure affords the crude product which is purified by column chromatography on silica gel.

후처리

  1. temperatureThe resulting solution is heated
  2. temperatureat reflux for 16 hours
  3. temperature
The reaction mixture is cooled with ice
  • customquenched with excess 2 N HCl
  • extractionextracted with methylene chloride
  • washThe combined extracts are washed with water
  • dry with materialdried with anhydrous magnesium sulfate
  • concentrationConcentration under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-2f9700ca58a84115ad1cc9a5d21dd3f1
    출처 데이터셋
    uspto-grants-1990_05
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04923885

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