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HCID 13186366, 화합물 → HCID 135816716, 화합물

HRID 1388301
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HRID 1388301 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[N:10]=[C:11]([CH2:14][S:15]([NH:18][C:19](=[O:25])[C:20](OCC)=[O:21])(=[O:17])=[O:16])[S:12][CH:13]=2)[CH:5]=[CH:6][C:7]=1[Cl:8].CC(C)([O-])C.[K+]>CN(C)C=O.O>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]2[N:10]=[C:11]([C:14]3[S:15](=[O:17])(=[O:16])[NH:18][C:19](=[O:25])[C:20]=3[OH:21])[S:12][CH:13]=2)[CH:5]=[CH:6][C:7]=1[Cl:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 13186366HCID 13186366, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 135816716HCID 135816716, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of the 2-thiazolylmethyl substituted oxamate intermediate prepared in Step B above (1.0 g., 0.0024 mol) in dimethylformamide (5 ml) was added potassium tert-butoxide (0.55 g, 0.0048 ml) in several portions over 15 minutes. The mixture was stirred at room temperature for 24 hours. After diluting with water (30 ml) and acidifying to congo red indicator paper, a yellow gum (1.1 g.) was obtained. Recrystallization was achieved by dissolving in boiling ether (500 ml), filtering, concentrating to a small volume, and adding petroleum ether. The yield of the title product was 0.3 g., m.p. 250° C. (dec.).

후처리

  1. customa yellow gum (1.1 g.) was obtained
  2. customRecrystallization
  3. dissolutionby dissolving
  4. filtrationfiltering
  5. concentrationconcentrating to a small volume
  6. additionadding petroleum ether

출처 및 근거

ORD 기록
ord-324758f573fe45e89ad51a03f20c6c08
출처 데이터셋
uspto-grants-1984_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04431652

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