Hydrochloric Acid → HCID 67497105、化合物

HRID 1628204ノート

反応式

HRID 1628204 の反応式
[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]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 69620697HCID 69620697、化合物

生成物 1

HCID 67497105HCID 67497105、化合物収率 85%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

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%)

後処理

  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

出典と根拠

ORDレコード
ord-8a439034a03349bcab7b7bb3d210e04f
出典データセット
uspto-grants-2014_07
特許番号
US08785468B2

反応ノート

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