Hydrochloric Acid → HCID 69458120、化合物

HRID 1351964ノート

反応式

HRID 1351964 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([C@H:8]2[O:12][C:11](=[O:13])[N:10]([C@H:14]([CH3:33])[CH2:15][C:16]3[C:24]4[C:19](=[C:20]([NH:25]C(=O)OC(C)(C)C)[CH:21]=[CH:22][CH:23]=4)[NH:18][CH:17]=3)[CH2:9]2)[CH:5]=[CH:6][CH:7]=1.Cl>CO>[NH2:25][C:20]1[CH:21]=[CH:22][CH:23]=[C:24]2[C:19]=1[NH:18][CH:17]=[C:16]2[CH2:15][C@H:14]([N:10]1[CH2:9][C@@H:8]([C:4]2[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=2)[O:12][C:11]1=[O:13])[CH3:33]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 69458797HCID 69458797、化合物

生成物 1

HCID 69458120HCID 69458120、化合物収率 90.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

To a solution of tert-butyl 3-((2R)-2-((5R)-5-(3-chlorophenyl)-2-oxo-1,3-oxazolidin-3-yl)propyl)-1H-indol-7-ylcarbamate (419.2 mg, 0.894 mmol) in methanol (2 mL) is added a 10% solution of hydrochloric acid in methanol (10 mL) under nitrogen atmosphere, and the mixture is stirred at room temperature for 21 hours. The solvent is evaporated, and the residue is separated into a saturated ammonia solution in chloroform and water, and the organic layer is washed with a saturated brine, and dried over anhydrous sodium sulfate. The solvent is evaporated, and the obtained crude product is purified by silica gel column chromatography (a saturated ammonia solution in chloroform-methanol=1:0 20:1) to give the title compound (299 mg, 90%).

後処理

  1. customThe solvent is evaporated
  2. customthe residue is separated into a saturated ammonia solution in chloroform and water
  3. washthe organic layer is washed with a saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent is evaporated
  6. customthe obtained crude product
  7. customis purified by silica gel column chromatography (a saturated ammonia solution in chloroform-methanol=1:0 20:1)

出典と根拠

ORDレコード
ord-6eebcda1781a430484f4a3a5903af440
出典データセット
uspto-grants-2007_05
特許番号
US07217724B2

反応ノート

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