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Hydrochloric Acid → HCID 135773208, 화합물

HRID 904693
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HRID 904693 반응식
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([CH2:15][CH2:16][CH3:17])[C:13]=1[OH:14])[N:10]=[C:9]([C:18]([OH:20])=[O:19])[CH:8]=[C:7]2[NH:21][CH2:22][CH3:23])(=[O:3])[CH3:2].Cl.O.[CH2:26](O)[CH3:27]>>[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[C:12]([CH2:15][CH2:16][CH3:17])[C:13]=1[OH:14])[N:10]=[C:9]([C:18]([O:20][CH2:26][CH3:27])=[O:19])[CH:8]=[C:7]2[NH:21][CH2:22][CH3:23])(=[O:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 135773200HCID 135773200, 화합물

생성물 1

HCID 135773208HCID 135773208, 화합물

실험 절차

The product of step (a) in ethanol was saturated with hydrogen chloride gas and, when the heat of solvation subsided, the brown solution was heated to reflux on a steambath for 5 hours. The mixture was cooled and was treated with water, then concentrated and the pH of the mixture was adjusted to about 7 before extracting into ethyl acetate. The extract was washed with water, dried and evaporated to give a yellowish solid (6.2 g; 82%). NMR and mass spectra were consistent with the required structure.

후처리

  1. temperatureheat of solvation
  2. temperaturethe brown solution was heated
  3. temperatureto reflux on a steambath for 5 hours
  4. temperatureThe mixture was cooled
  5. concentrationconcentrated
  6. extractionbefore extracting into ethyl acetate
  7. washThe extract was washed with water
  8. customdried
  9. customevaporated
  10. customto give a yellowish solid (6.2 g; 82%)

출처 및 근거

ORD 기록
ord-894491307224456f9ed7cc44adad19ac
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04419352

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