Sodium Glycinate → HCID 178422967、化合物

HRID 1746187ノート

反応式

HRID 1746187 の反応式
CO[C:3]([C:5]1[C:6](=[O:17])[S:7][C:8]2[C:13]([C:14]=1[OH:15])=[CH:12][CH:11]=[C:10]([CH3:16])[CH:9]=2)=[O:4].[NH2:18][CH2:19][C:20]([O-:22])=[O:21].[Na+]>COCCO>[OH:15][C:14]1[C:13]2[C:8](=[CH:9][C:10]([CH3:16])=[CH:11][CH:12]=2)[S:7][C:6](=[O:17])[C:5]=1[C:3]([NH:18][CH2:19][C:20]([OH:22])=[O:21])=[O:4]

参加物

4

反応物 2

HCID 4684308Sodium GlycinateHCID 178498939HCID 178498939、化合物

生成物 1

HCID 178422967HCID 178422967、化合物収率 94.8%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

A mixture of 4-hydroxy-7-methyl-2-oxo-2H-thiochromene-3-carboxylic acid methyl ester (80 mg, 0.32 mmol) and sodium glycinate (310 mg, 3.2 mmol) in 2-methoxyethanol (10 mL) was refluxed for 3 h. The reaction mixture was concentrated and the crude residue dissolved in water (50 mL), acidified to pH 3-4 using 1 N HCl and extracted with EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated to provide [(4-hydroxy-7-methyl-2-oxo-2H-thiochromene-3-carbonyl)-amino]-acetic acid (89 mg). MS ESI(−) m/e: 292.12 (M−1).

後処理

  1. temperaturewas refluxed for 3 h
  2. concentrationThe reaction mixture was concentrated
  3. dissolutionthe crude residue dissolved in water (50 mL)
  4. extractionextracted with EtOAc
  5. washThe organic layer was washed with brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-4da05eece0c849b58f811537a00ec1d2
出典データセット
uspto-grants-2015_10
特許番号
US09149476B2

反応ノート

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