Acetic Acid → HCID 20338069, 화합물

HRID 1395761노트

반응식

HRID 1395761 반응식
[O:1]=[C:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[N:12][C:6]=2[S:5][C:4]2[CH:13]=[CH:14][C:15]([CH:17]([CH3:21])[C:18]([OH:20])=[O:19])=[CH:16][C:3]1=2.[N+](=[CH2:24])=[N-].C(O)(=O)C.C(=O)([O-])O.[Na+]>C(O)C>[O:1]=[C:2]1[CH2:8][C:7]2[CH:9]=[CH:10][CH:11]=[N:12][C:6]=2[S:5][C:4]2[CH:13]=[CH:14][C:15]([CH:17]([CH3:21])[C:18]([O:20][CH3:24])=[O:19])=[CH:16][C:3]1=2

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 9550DiazomethaneHCID 516892Sodium BicarbonateHCID 20506969HCID 20506969, 화합물

생성물 1

HCID 20338069HCID 20338069, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To 54 mg of 2-(5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]-thiepin-8-yl)-propionic acid in ethanol was added 5 ml of diazomethane etherial solution and the mixture was stirred at room temperature for 1 hour. To this was added acetic acid to decompose an excess reagent, then saturated sodium hydrogen-carbonate solution to make the solution alkaline, and the mixture was extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was distilled off to obtain 51 mg of oily substance, which was chromatographed over silica gel, eluted with benzene/chloroform (1/1) to obtain the colorless oily substance, which was crystallized from ethanol to give 40 mg of methyl 2-(5,6-dihydro-6-oxo benzo[b]pyrido[3,2-f]thiepin-8-yl)-propionate as colorless crystals having a melting point of 98°-99.5° C.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated sodium chloride solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off
  5. customto obtain 51 mg of oily substance, which
  6. customwas chromatographed over silica gel
  7. washeluted with benzene/chloroform (1/1)
  8. customto obtain the colorless oily substance, which
  9. customwas crystallized from ethanol

출처 및 근거

ORD 기록
ord-ec3b34796d6d4a4798abcbcb6f80dc9f
출처 데이터셋
uspto-grants-1980_05
특허 번호
US04205170

반응 노트

불러오는 중…