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HCID 72644370, 화합물 → HCID 72644365, 화합물

HRID 1581644
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HRID 1581644 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 72644370HCID 72644370, 화합물

생성물 1

HCID 72644365HCID 72644365, 화합물수율 50.2%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b36b050e7f6c408e86b70ed8f9e10a34
출처 데이터셋
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06730687B1

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