Hydrochloric Acid → HCID 10474189、化合物

HRID 1793823ノート

反応式

HRID 1793823 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]([C:13]2[CH:18]=[C:17]([OH:19])[C:16]([O:20][CH3:21])=[CH:15][C:14]=2[CH:22]([CH2:26][CH3:27])[C:23](=O)[CH3:24])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[NH2:28][NH2:29].Cl>C(O)C>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C:13]3[CH:18]=[C:17]([OH:19])[C:16]([O:20][CH3:21])=[CH:15][C:14]=3[CH:22]([CH2:26][CH3:27])[C:23]([CH3:24])=[N:29][N:28]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9321HydrazineHCID 222197323-[2-(3,4-Dimethoxybenzoyl)-4-hydroxy-5-methoxyphenyl]pentan-2-one

生成物 1

HCID 10474189HCID 10474189、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 14 g of 3-{2-[(3,4-dimethoxyphenyl)carbonyl]-4-hydroxy-5-methoxyphenyl}pentan-2-one and 4.7 mL of hydrazine in 280 mL of ethanol was heated at reflux for 0.5 hr. After allowing the solution to cool to room temperature, it was saturated with HCl gas. The mixture was then concentrated to a volume of about 5 mL, basified with concentrated ammonium hydroxide, and extracted with methylene chloride. The combined methylene chloride extracts were dried and concentrated, and the residue recrystallized from ethyl acetate/hexane. Yield: 1.5 g

後処理

  1. temperatureat reflux for 0.5 hr
  2. concentrationThe mixture was then concentrated to a volume of about 5 mL
  3. extractionextracted with methylene chloride
  4. dry with materialThe combined methylene chloride extracts were dried
  5. concentrationconcentrated
  6. customthe residue recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-cf908bae29b7404681d8111d8162a2a9
出典データセット
uspto-grants-2006_04
特許番号
US07022700B2

反応ノート

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