Water → HCID 59407289、化合物

HRID 1455525ノート

反応式

HRID 1455525 の反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6](=[O:9])[N:5]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[C:4]=1[S-:16])#[N:2].[Na+].Br[CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21].O>CCO>[CH2:23]([O:22][C:20]([C:19]1[S:16][C:4]2[N:5]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:6](=[O:9])[CH:7]=[CH:8][C:3]=2[C:1]=1[NH2:2])=[O:21])[CH3:24]

参加物

5

反応物 3

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 11615758Sodium 3-cyano-6-oxo-1-phenyl-1,6-dihydropyridine-2-thiolate

生成物 1

HCID 59407289HCID 59407289、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of Example 1 (0.34 g at 100%) and ethyl bromoacetate (0.197 mL) in EtOH (6 mL) was stirred at room temperature for 1 h. H2O (10 mL) was then added. The solid was filtered and washed with more H2O (2 mL). The product was dried under vacuum at 40° C. to constant weight to give the title compound as a pale pink solid (0.35 g). δH (DMSO-d6) 8.20 (1H, d, J 9.6 Hz), 7.60 (3H, m), 7.45 (2H, m), 7.15 (2H, br s), 6.55 (1H, d, J 9.6 Hz), 4.15 (2H, q, J 7.1 Hz), 1.20 (3H, t, J 7.1 Hz). LCMS (ES+) RT 3.29 minutes, 315 (M+H)+.

後処理

  1. filtrationThe solid was filtered
  2. washwashed with more H2O (2 mL)
  3. customThe product was dried under vacuum at 40° C. to constant weight

出典と根拠

ORDレコード
ord-0a006cdd58fe458788a7ce0fe02ccd27
出典データセット
uspto-grants-2009_01
特許番号
US07482452B2

反応ノート

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