Acetone → Sodium 5-(1,1-dioxido-1,2-thiazinan-2-yl)-7-[({4-fluoro-2-[(methylamino)carbonyl]benzyl}amino)carbonyl]-1,6-naphthyridin-8-olate

HRID 2252805ノート

反応式

HRID 2252805 の反応式
[OH-].[Na+:2].[O:3]=[S:4]1(=[O:36])[CH2:9][CH2:8][CH2:7][CH2:6][N:5]1[C:10]1[N:19]=[C:18]([C:20]([NH:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=2[C:31]([NH:33][CH3:34])=[O:32])=[O:21])[C:17]([OH:35])=[C:16]2[C:11]=1[CH:12]=[CH:13][CH:14]=[N:15]2.CC(C)=O.C(#N)C>O>[O:36]=[S:4]1(=[O:3])[CH2:9][CH2:8][CH2:7][CH2:6][N:5]1[C:10]1[N:19]=[C:18]([C:20]([NH:22][CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][C:25]=2[C:31]([NH:33][CH3:34])=[O:32])=[O:21])[C:17]([O-:35])=[C:16]2[C:11]=1[CH:12]=[CH:13][CH:14]=[N:15]2.[Na+:2]

参加物

6

反応物 4

HCID 180AcetoneHCID 6342AcetonitrileHCID 14798Sodium HydroxideHCID 30133965-(1,1-dioxothiazinan-2-yl)-N-[[4-fluoro-2-(methylcarbamoyl)phenyl]methyl]-8-hydroxy-1,6-naphthyridine-7-carboxamide

生成物 1

HCID 69180949Sodium 5-(1,1-dioxido-1,2-thiazinan-2-yl)-7-[({4-fluoro-2-[(methylamino)carbonyl]benzyl}amino)carbonyl]-1,6-naphthyridin-8-olate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium hydroxide (150 μL, 0.15 mmol, 1N solution) was added to a cloudy solution of 5-(1,1-dioxido-1,2-thiazinan-2-yl)-N-{4-fluoro-2-[(methylamino)carbonyl]benzyl}-8-hydroxy-1,6-naphthyridine-7-carboxamide (73 mg, 0.15 mmol) in a 2 mL mixture of acetone, acetonitrile and water. The homogeneous bright yellow solution was allowed to stir at room temperature for 30 minutes. The solvent was removed in vacuo and dried overnight on the high vac with gentle heating to give the desired product as a bright yellow solid.

後処理

  1. customThe solvent was removed in vacuo
  2. customdried overnight on the high vac
  3. temperaturewith gentle heating

出典と根拠

ORDレコード
ord-d64a7d43a37143dfacef00793149710a
出典データセット
uspto-grants-2008_01
特許番号
US07323460B2

反応ノート

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