Methylamine → 6-(Benzene sulfonyl amino-methyl)-3-benzyloxy-1-methyl-4-oxo-1,4-dihydro-pyridine-2-carboxylic acid

HRID 1846838ノート

反応式

HRID 1846838 の反応式
[C:1]1([S:7]([CH:10]([NH2:29])[C:11]2O[C:15]([C:17]([OH:19])=[O:18])=[C:14]([O:20][CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:13](=[O:28])[CH:12]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:30][NH2:31]>CO>[C:1]1([S:7]([CH:10]([NH2:29])[C:11]2[N:31]([CH3:30])[C:15]([C:17]([OH:19])=[O:18])=[C:14]([O:20][CH2:21][C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:13](=[O:28])[CH:12]=2)(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

4

反応物 2

HCID 6329MethylamineHCID 867256956-(benzene sulfonyl amino-methyl)-3-benzyloxy-4-oxo-4H-pyran-2-carboxylic acid

生成物 1

HCID 867256966-(Benzene sulfonyl amino-methyl)-3-benzyloxy-1-methyl-4-oxo-1,4-dihydro-pyridine-2-carboxylic acid収率 65.08%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of 6-(benzene sulfonyl amino-methyl)-3-benzyloxy-4-oxo-4H-pyran-2-carboxylic acid (12-01) (640.0 mg, 1.54 mmol) in MeOH (5.0 mL) was added methylamine (2 M in methanol, 2.0 mL) at room temperature and the mixture was stirred for 6 h at room temperature. After completion of the reaction, the solvent was removed under reduced pressure to get the crude compound. It was then purified using normal column chromatography to get 6-(benzene sulfonyl amino-methyl)-3-benzyloxy-1-methyl-4-oxo-1,4-dihydro-pyridine-2-carboxylic acid (13-01) (430.0 mg, 65.08%) as a yellow solid.

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was removed under reduced pressure
  3. customto get the crude compound
  4. customIt was then purified

出典と根拠

ORDレコード
ord-3dafafba2ed348fa8dff6688e0d65a7c
出典データセット
uspto-grants-2015_02
特許番号
US08952039B2

反応ノート

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