Hydrochloric Acid → 6-Hydroxy-1,3-dioxaindane-5-carbaldehyde

HRID 2364916ノート

反応式

HRID 2364916 の反応式
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7]([OH:10])[CH:8]=[CH:9][C:3]=2[O:2]1.C1N2CN3CN(C2)CN1C3.Cl.FC(F)(F)[C:24](O)=[O:25]>>[OH:10][C:7]1[C:8]([CH:24]=[O:25])=[CH:9][C:3]2[O:2][CH2:1][O:5][C:4]=2[CH:6]=1

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 68289Sesamol

生成物 1

HCID 67106266-Hydroxy-1,3-dioxaindane-5-carbaldehyde

実験手順

In a 500 mL recovery flask, 10.0 g (72.4 mmol) of sesamol (manufactured by Tokyo Chemical Industry Co., Ltd.) and 15.2 g (109 mmol, 1.5 eq) of hexamethylenetetramine (manufactured by Tokyo Chemical Industry Co., Ltd.) were dissolved in 100 ml of trifluoroacetic acid (manufactured by Kanto Chemical Co., Inc.) and reacted at 95° C. for 10 hours. After the reaction was completed, in an ice bath, 200 ml of 1 N hydrochloric acid was added thereto and the resultant was stirred for minutes. After the stirring was completed, the resultant was extracted with chloroform to obtain an extract. The extract was washed with hydrochloric acid and saturated saline, thereby obtaining 2.38 g (14.3 mmol) of 6-hydroxy-3,4-methylenedioxybenzaldehyde.

後処理

  1. customreacted at 95° C. for 10 hours
  2. customAfter the reaction was completed, in an ice bath
  3. extractionthe resultant was extracted with chloroform
  4. customto obtain an extract
  5. washThe extract was washed with hydrochloric acid and saturated saline

出典と根拠

ORDレコード
ord-1a60e20935924db8928e9e6dde723467
出典データセット
uspto-grants-2014_04
特許番号
US08697332B2

反応ノート

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