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Hydrochloric Acid → HCID 135773208、化合物

HRID 904693
ノート
印刷プレビュー

反応式

HRID 904693 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 135773200HCID 135773200、化合物

生成物 1

HCID 135773208HCID 135773208、化合物

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-894491307224456f9ed7cc44adad19ac
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04419352

反応ノート

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