Hydrochloric Acid → HCID 67497105, 화합물

HRID 1628204노트

반응식

HRID 1628204 반응식
[O:1]=[C:2]([NH:19][C:20]1[N:21]=[C:22]([C:25]2[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=2)[S:23][CH:24]=1)[C@@H:3]([NH:11]C(=O)OC(C)(C)C)[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.C([O-])(O)=O.[Na+]>O1CCOCC1.O>[NH2:11][C@@H:3]([CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[C:2]([NH:19][C:20]1[N:21]=[C:22]([C:25]2[CH:30]=[CH:29][N:28]=[CH:27][CH:26]=2)[S:23][CH:24]=1)=[O:1]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 69620697HCID 69620697, 화합물

생성물 1

HCID 67497105HCID 67497105, 화합물수율 85%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

To a rt solution of 4.B (163 mg, 384 μmol) in dioxane (2.5 mL) was added 6.0 N HCl (1 mL). After stirring at rt for 30 min, the reaction mixture was poured into saturated aqueous NaHCO3 (5 m L), diluted with water (5 mL) and extracted by 30% iPrOH/CHCl3 (3×10 mL). The combined solution was washed with brine and dried over MgSO4. After removal of organic solvent under reduced pressure, purification of the residue by flash chromatography on silica gel using 0-20% MeOH/CH2Cl2 for elution provided 4.C as a colorless solid (105 mg, 85%)

후처리

  1. extractionextracted by 30% iPrOH/CHCl3 (3×10 mL)
  2. washThe combined solution was washed with brine
  3. dry with materialdried over MgSO4
  4. customAfter removal of organic solvent
  5. customunder reduced pressure, purification of the residue by flash chromatography on silica gel using 0-20% MeOH/CH2Cl2
  6. washfor elution

출처 및 근거

ORD 기록
ord-8a439034a03349bcab7b7bb3d210e04f
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785468B2

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