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HCID 72644370、化合物 → HCID 72644365、化合物

HRID 1581644
ノート
印刷プレビュー

反応式

HRID 1581644 の反応式
CS[CH:3]([C:9]1[CH:14]=[C:13]([CH:15]=[C:16]2[S:20][C:19](=[O:21])[NH:18][C:17]2=[O:22])[CH:12]=[CH:11][C:10]=1[O:23][CH3:24])[C:4]([O:6][CH2:7][CH3:8])=[O:5]>[Zn].C(O)(=O)C>[O:21]=[C:19]1[NH:18][C:17](=[O:22])[C:16](=[CH:15][C:13]2[CH:12]=[CH:11][C:10]([O:23][CH3:24])=[C:9]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])[CH:14]=2)[S:20]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 1

HCID 72644370HCID 72644370、化合物

生成物 1

HCID 72644365HCID 72644365、化合物収率 50.2%

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 176Acetic Acid溶媒

実験手順

Ethyl 2-methylthio-2-[5-[(2,4-dioxothiazolidin-5-ylidene)methyl]-2-methoxyphenyl]acetate (6.18 g, 16.8 mmol) and acetic acid (100 mL) were mixed, and zinc powder (46.0 g, 706 mmol) was added under stirring, which was stirred for 24 hours at room temperature. Zinc was collected by filtration. washed with acetic acid, and the filtrate was concentrated. The residue was dissolved into ethyl acetate, washed with water and brine in sequence, then dried over anhydrous sodium sulfate and concentrated. The residue was recrystallized from methanol to obtain 2.71 g (50%) of the title compound as yellow powder.

後処理

  1. stirringwhich was stirred for 24 hours at room temperature
  2. filtrationZinc was collected by filtration
  3. washwashed with acetic acid
  4. concentrationthe filtrate was concentrated
  5. dissolutionThe residue was dissolved into ethyl acetate
  6. washwashed with water and brine in sequence
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated
  9. customThe residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-b36b050e7f6c408e86b70ed8f9e10a34
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06730687B1

反応ノート

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