Ammonium Chloride → HCID 21834217、化合物

HRID 231493ノート

反応式

HRID 231493 の反応式
[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

参加物

6

反応物 3

HCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 57199523HCID 57199523、化合物

生成物 1

HCID 21834217HCID 21834217、化合物

試薬・触媒・溶媒 2

HCID 78391,2-Dibromoethane触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-629bf9864f8d42f5a0181eb5b1722e9b
出典データセット
uspto-grants-1989_07
特許番号
US04847254

反応ノート

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