Ammonium Chloride → HCID 21834217, 화합물

HRID 231493노트

반응식

HRID 231493 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH:8]=[C:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1.[Mg].[Cl-].[NH4+]>CO.BrCCBr>[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[S:9][CH2:8][CH:7]([C:10]([N:12]([CH2:16][CH2:17][CH3:18])[CH2:13][CH2:14][CH3:15])=[O:11])[C:6]=2[CH:19]=1

참가 물질

6

반응물 3

HCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 57199523HCID 57199523, 화합물

생성물 1

HCID 21834217HCID 21834217, 화합물

시약·촉매·용매 2

HCID 78391,2-Dibromoethane촉매HCID 887Methanol용매

실험 절차

30 g of 5-amino-N,N-dipropyl-3-benzothiophencarboxamide were dissolved in 250 ml of dry methanol. 15 g of magnesium turnings were added (eventually activated by addition of a few drops of 1,2-dibromoethane). The mixture was stirred at 30°-35° C. for 4 hours with periodically cooling to keep the temperature down. 2 l of a saturated ammonium chloride solution were added and the product extracted with ethyl acetate. The organic phase was separated, washed with water, dried (MgSO4) and the solvent evaporated. Isopropyl ether was added, and by cooling the title compound precipitated and was filtered off. Yield: 20 g. M.P. 100° C.

후처리

  1. temperaturewith periodically cooling
  2. extractionthe product extracted with ethyl acetate
  3. customThe organic phase was separated
  4. washwashed with water
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated
  7. additionIsopropyl ether was added
  8. temperatureby cooling the title compound
  9. customprecipitated
  10. filtrationwas filtered off

출처 및 근거

ORD 기록
ord-629bf9864f8d42f5a0181eb5b1722e9b
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04847254

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