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Sodium Carbonate → HCID 178503549、化合物

HRID 2353640
ノート
印刷プレビュー

反応式

HRID 2353640 の反応式
S(O)(O)(=O)=O.[CH3:6][S:7][C:8](=[NH:10])[NH2:9].[Cl:11][CH2:12][C:13](=O)[CH2:14][C:15](OCC)=[O:16].C(=O)([O-])[O-].[Na+].[Na+]>O>[Cl:11][CH2:12][C:13]1[N:9]=[C:8]([S:7][CH3:6])[N:10]=[C:15]([OH:16])[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 69484Ethyl 4-chloroacetoacetateHCID 752702-Methyl-2-thiopseudourea sulfate

生成物 1

HCID 178503549HCID 178503549、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

S-Methyl-2-thiopseudourea sulphate (20 g, 71.85 mmol), ethyl 4-chloroacetoacetate (10.755 ml, 79.04 mmol) and sodium carbonate (13.925 g, 107.78 mmol) were dissolved in water (100 ml) and stirred at room temperature overnight. The reaction was monitored by TLC, and once complete, the reaction precipitate was collected and the supernatant was neutralised with 6N hydrochloric acid to yield more reaction precipitate which was also collected. The accumulated precipitate was then washed with water (×3) and an off-white solid was obtained. This was dried in vacuo at 60° C. for 48 hours to yield the desired compound as a pale yellow/white solid, 43.2 g.

後処理

  1. customonce complete, the reaction precipitate was collected
  2. customto yield more
  3. customreaction precipitate which
  4. customwas also collected
  5. washThe accumulated precipitate was then washed with water (×3)
  6. customan off-white solid was obtained
  7. customThis was dried in vacuo at 60° C. for 48 hours

出典と根拠

ORDレコード
ord-2115342f0cbd4b5a95e8a6005d9214d3
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750003B2

反応ノート

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