Sodium Methoxide → (3-Bromo-5-iodophenyl)-thiourea

HRID 1941921ノート

反応式

HRID 1941921 の反応式
C([NH:9][C:10]([NH:12][C:13]1[CH:18]=[C:17]([I:19])[CH:16]=[C:15]([Br:20])[CH:14]=1)=[S:11])(=O)C1C=CC=CC=1.C[O-].[Na+]>CO>[Br:20][C:15]1[CH:14]=[C:13]([NH:12][C:10]([NH2:9])=[S:11])[CH:18]=[C:17]([I:19])[CH:16]=1

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 578136521-Benzoyl-3-(3-bromo-5-iodophenyl)-thiourea

生成物 1

HCID 57813682(3-Bromo-5-iodophenyl)-thiourea収率 89.5%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A stirred suspension of 1-Benzoyl-3-(3-bromo-5-iodophenyl)-thiourea (20.70 g, 0.0449 mol) in methanol (303 ml) was treated with sodium methoxide (2.42 g, 0.0449 mol) and stirred at ambient temperature for 4 h. The resultant suspension was evaporated to dryness at reduced pressure. The residue was mixed with water (500 ml) and extracted with ethyl acetate (3×200 ml) which was dried (MgSO4) and the solvent removed in vacuo to give a residue which was triturated with 40-60° petroleum ether/diethyl ether (1:1) to afford (3-Bromo-5-iodophenyl)-thiourea as an off-white solid (14.35 g, 89%).

後処理

  1. customThe resultant suspension was evaporated to dryness at reduced pressure
  2. additionThe residue was mixed with water (500 ml)
  3. extractionextracted with ethyl acetate (3×200 ml) which
  4. dry with materialwas dried (MgSO4)
  5. customthe solvent removed in vacuo
  6. customto give a residue which
  7. customwas triturated with 40-60° petroleum ether/diethyl ether (1:1)

出典と根拠

ORDレコード
ord-ba3ff37c1de14d72809550f7fa5c536d
出典データセット
uspto-grants-2013_03
特許番号
US08389516B2

反応ノート

読み込み中…