Sodium Hydroxide → 1-(3-(Benzyloxy)-5-bromopyridin-2-yl)thiourea

HRID 1426082ノート

反応式

HRID 1426082 の反応式
C([NH:9][C:10]([NH:12][C:13]1[C:18]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:17][C:16]([Br:27])=[CH:15][N:14]=1)=[S:11])(=O)C1C=CC=CC=1.[OH-].[Na+]>O>[CH2:20]([O:19][C:18]1[C:13]([NH:12][C:10]([NH2:9])=[S:11])=[N:14][CH:15]=[C:16]([Br:27])[CH:17]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 866396501-Benzoyl-3-(3-(benzyloxy)-5-bromopyridin-2-yl)thiourea

生成物 1

HCID 727056401-(3-(Benzyloxy)-5-bromopyridin-2-yl)thiourea収率 92.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A 1 L round-bottom flask was charged with 1-benzoyl-3-(3-(benzyloxy)-5-bromopyridin-2-yl)thiourea (17.9 g, 40.5 mmol) and 3M sodium hydroxide (3.3 mL, 9.9 mmol), and the reaction mixture was refluxed overnight. The reaction mixture was then cooled, poured into water, and filtered to provide 1-(3-(benzyloxy)-5-bromopyridin-2-yl)thiourea (12.6 g, 92.2% yield) as a yellow solid. 1H NMR (CDCl3) δ 10.60 (bs, 1H), 8.59 (bs, 1H), 7.87 (d, 1H), 7.40 (m, 5H), 7.30 (d, 1H), 6.90 (m, 1H), 5.15 (s, 2H). Mass spectrum (apci) m/z=340.0 (M+H).

後処理

  1. temperaturethe reaction mixture was refluxed overnight
  2. temperatureThe reaction mixture was then cooled
  3. filtrationfiltered

出典と根拠

ORDレコード
ord-8fc37007cb4b49b8be39c803ddc45e07
出典データセット
uspto-grants-2015_01
特許番号
US08933077B2

反応ノート

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