Hydrochloric Acid → 5,6-Dimethoxy-3H-isobenzofuran-1-one

HRID 1060576

反応式

HRID 1060576 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6]([OH:8])=[O:7].[CH2:14]=O.Cl>Cl>[CH3:13][O:12][C:11]1[CH:10]=[C:9]2[C:5](=[CH:4][C:3]=1[O:2][CH3:1])[C:6](=[O:8])[O:7][CH2:14]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 712FormaldehydeHCID 7121Veratric Acid

生成物 1

HCID 2304605,6-Dimethoxy-3H-isobenzofuran-1-one収率 58.65%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid触媒

実験手順

A suspension of 3,4-dimethoxy-benzoic acid (353.5 g, 1.94 moles) in HCHO (1.7 l, 24.5 moles) was prepared under mechanic stirring, cooled in ice, saturated with gaseous HCl (340 g, 9.32 moles), then gradually brought to 60° C. After one night the temperature was brought to the room values and further HCl (300 mg) was bubbled, then the temperature was brought again to 60° C. for one night. The mixture was brought to small volume, taken up with water (1 l ), neutralised with 28% NH4OH (1.5 l) and kept at cool for 2 hours, then filtered. The filtrate was washed with water up to neutrality, then crystallised from CH3OH (2 l ) and dried under vacuum at 60° C. to give 220 g of the title compound (yield: 58.65%).

後処理

  1. customwas prepared under mechanic stirring
  2. customgradually brought to 60° C
  3. customwas bubbled
  4. waitthe temperature was brought again to 60° C. for one night
  5. temperatureat cool for 2 hours
  6. filtrationfiltered
  7. washThe filtrate was washed with water up to neutrality
  8. customcrystallised from CH3OH (2 l )
  9. customdried under vacuum at 60° C.

出典と根拠

ORDレコード
ord-8f4989f60dc24bcb91078e1fc2241646
出典データセット
uspto-grants-2003_02
特許番号
US06525055B1

関連ノート

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