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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → HCID 178492000, 화합물

HRID 1244318
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인쇄 미리보기

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HRID 1244318 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:5][C:4]=1[NH:15][C:16]([C:18]1[NH:27][C:21]2=[N:22][C:23]([CH3:26])=[CH:24][CH:25]=[C:20]2[N:19]=1)=[S:17].Br.CC(O)=O.CS(C)=O.[OH-].[NH4+]>C(OCC)(=O)C.O>[CH3:1][O:2][C:3]1[C:4]2[N:15]=[C:16]([C:18]3[NH:27][C:21]4=[N:22][C:23]([CH3:26])=[CH:24][CH:25]=[C:20]4[N:19]=3)[S:17][C:5]=2[C:6]([N:9]2[CH2:10][CH2:11][O:12][CH2:13][CH2:14]2)=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 679Dimethyl SulfoxideHCID 14923Ammonium HydroxideHCID 178492018HCID 178492018, 화합물

생성물 1

HCID 178492000HCID 178492000, 화합물수율 42%

시약·촉매·용매 2

HCID 962
Water
용매
2회
HCID 8857Ethyl Acetate용매

실험 절차

0.3 g 5-Methyl-3H-imidazo[4,5-b]pyridine-2-carbothioic acid (2-methoxy-5-morpholin-4-yl-phenyl)-amide (0.8 mmol) was dissolved in ethyl acetate (3 ml), heated to reflux and treated with 0.27 ml HBr in AcOH (5.7M, 1.6 mmol) and 0.067 ml DMSO (0.94 mmol). Stirring at reflux was continued for 2 h. Upon cooling a precipitation formed, which was isolated and dissolved in water (2 ml). The pH was adjusted to 10 with 25% ammonium hydroxide in water. Once again a precipitation formed, which was filtered. The residue on the filter was washed with water and dried in vacuo. One obtained 0.125 g 2-(4-methoxy-7-morpholin-4-yl-benzothiazol-2-yl)-5-methyl-3H-imidazo[4,5-b]pyridine (42%) as a yellow solid; M.p.: 200–210° C.

후처리

  1. temperatureheated
  2. temperatureto reflux
  3. temperatureat reflux
  4. temperatureUpon cooling
  5. customa precipitation
  6. customformed
  7. customwhich was isolated
  8. customOnce again a precipitation
  9. customformed
  10. filtrationwhich was filtered
  11. washThe residue on the filter was washed with water
  12. customdried in vacuo

출처 및 근거

ORD 기록
ord-ae3b39c27c874c67b567bbd06fafeeb3
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07122545B2

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