Hydrochloric Acid → HCID 86663294、化合物

HRID 2364918ノート

反応式

HRID 2364918 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([OH:10])[CH:5]=[CH:6][C:7]=1[N:8]=[O:9].C1N2CN3CN(C2)CN1C3.Cl.FC(F)(F)[C:24](O)=[O:25]>>[OH:10][C:4]1[CH:3]=[C:2]([CH3:1])[C:7]([N:8]=[O:9])=[CH:6][C:5]=1[CH:24]=[O:25]

参加物

5

反応物 4

HCID 313Hydrochloric AcidHCID 4101HexamethylenetetramineHCID 6422Trifluoroacetic acidHCID 119814-Nitroso-3-methylphenol

生成物 1

HCID 86663294HCID 86663294、化合物

実験手順

In a 500 mL recovery flask, 5.0 g (36.5 mmol) of 3-methyl-4-nitrosophenol (manufacture by Aldrich Inc.) and 7.63 g (54.7 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 15 minutes. After the stirring, the resultant was extracted with chloroform to obtain an extract. The extract was washed with hydrochloric acid and unsaturated saline, thereby obtaining 1.51 g (9.13 mmol) of 2-hydroxy-4-methyl-5-nitroso-benzaldehyde.

後処理

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

出典と根拠

ORDレコード
ord-fa8f6d1729be43beaf7462ef68863f10
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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