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Dimethylamine → HCID 21836659, 화합물

HRID 1740217
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HRID 1740217 반응식
O1CCCCC1[O:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[N:21]=[C:22]=[O:23])=[CH:11][CH:10]=1.[CH3:24][NH:25][CH3:26]>CO>[OH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[NH:21][C:22]([N:25]([CH3:26])[CH3:24])=[O:23])=[CH:11][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 21836704HCID 21836704, 화합물

생성물 1

HCID 21836659HCID 21836659, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of the crude intermediate from Step A in 4 mL of methanol was treated with 4 mL of 40% aqueous dimethylamine. After stirring at room temperature for 15 minutes, the reaction mixture was evaporated under vacuum and the residue dissolved in 4 mL of methanol and treated with 1 mL of 10% methanolic p-toluenesulfonic acid. After 15 minutes at room temperature, the reaction mixture was treated with saturated aqueous sodium bicarbonate. The mixture was diluted with water then extracted with methylene chloride. The organic layer was dried and evaporated under vacuum; the residue was purified by preparative thin layer chromatography on silica gel, eluting with hexane/ethyl acetate (2:1) to afford 133 mg of product.

후처리

  1. customthe reaction mixture was evaporated under vacuum
  2. dissolutionthe residue dissolved in 4 mL of methanol
  3. additiontreated with 1 mL of 10% methanolic p-toluenesulfonic acid
  4. waitAfter 15 minutes at room temperature
  5. additionthe reaction mixture was treated with saturated aqueous sodium bicarbonate
  6. additionThe mixture was diluted with water
  7. extractionthen extracted with methylene chloride
  8. customThe organic layer was dried
  9. customevaporated under vacuum
  10. customthe residue was purified by preparative thin layer chromatography on silica gel
  11. washeluting with hexane/ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-18e08fe0b62547c99d4a05f9ec6f1029
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05968924

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