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Thiourea → Ethyl 2-amino-4-(propan-2-yl)-1,3-thiazole-5-carboxylate

HRID 1660568
ノート
印刷プレビュー

反応式

HRID 1660568 の反応式
Cl[CH:2]([CH2:8][CH:9]([CH3:11])[CH3:10])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[NH2:12][C:13]([NH2:15])=[S:14]>C(O)C>[NH2:15][C:13]1[S:14][C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[C:8]([CH:9]([CH3:11])[CH3:10])[N:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2723790ThioureaHCID 20557029Ethyl 2-chloro-4-methylpentanoate

生成物 1

HCID 824436Ethyl 2-amino-4-(propan-2-yl)-1,3-thiazole-5-carboxylate収率 39.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Utilizing the procedure of Example 1, a mixture of 1.97 g (0.01 mol) of ethyl 2-chloro-4-methyl-pentanoate, 0.76 g (0.01 mol) of thiourea and 30 ml of ethanol was held at reflux for 18 hours. Ethanol was removed under reduced pressure. The residue was crystallized from hexane. The solid precipitates were dissolved in ether. The ether solution was washed with water, dried over magnesium sulfate and concentrated under reduced pressure. The residue was recrystallized from benzene-ether to give 0.85 g (39.6%) of ethyl 2-amino-4-isopropyl-5-thiazolecarboxylate, m.p. 173°-176° C.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperatureat reflux for 18 hours
  2. customEthanol was removed under reduced pressure
  3. customThe residue was crystallized from hexane
  4. customThe solid precipitates
  5. dissolutionwere dissolved in ether
  6. washThe ether solution was washed with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was recrystallized from benzene-ether

出典と根拠

ORDレコード
ord-031f732e532d47bab1a6100ae48e1a54
出典データセット
uspto-grants-1981_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04308391

反応ノート

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