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Methanol → N,N-dimethyl-1,2,3,4-tetrahydro-5-amino-8-hydroxyquinolinium bromide

HRID 918215
ノート
印刷プレビュー

反応式

HRID 918215 の反応式
[Br-:1].[CH3:2][N+:3]1([CH3:22])[C:12]2[C:7](=[C:8]([N:14]=NC3C=CC=CC=3)[CH:9]=[CH:10][C:11]=2[OH:13])[CH2:6][CH2:5][CH2:4]1.CO.[H][H]>[Pd].O>[Br-:1].[CH3:2][N+:3]1([CH3:22])[C:12]2[C:7](=[C:8]([NH2:14])[CH:9]=[CH:10][C:11]=2[OH:13])[CH2:6][CH2:5][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 136354588HCID 136354588、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 21521293N,N-dimethyl-1,2,3,4-tetrahydro-5-amino-8-hydroxyquinolinium bromide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

Into a stainless steel autoclave, one introduces 36.2 g of N,N-dimethyl-1,2,3,4-tetrahydro-5-phenylazo-8-hydroxyquinolinium bromide (i.e. 0.1 mole), 200 ml of methanol and 3 g of 5% palladium on charcoal. The reduction is carried out at a pressure of 3-5 kg/cm2 of hydrogen and a temperature of 50°-60°C. After cooling, one adds a sufficient quantity of water to dissolve the entire mass, then one filters off the catalyst. One evaporates the filtrate to the dry state. The residue is extracted by means of ether so as to remove the aniline. One washes, with acetone, the clear brown compound that is obtained.

後処理

  1. customa temperature of 50°-60°C
  2. temperatureAfter cooling
  3. dissolutionto dissolve the entire mass
  4. customOne evaporates the filtrate to the dry state
  5. extractionThe residue is extracted by means of ether so as
  6. customto remove the aniline
  7. customOne washes, with acetone, the clear brown compound that is obtained

出典と根拠

ORDレコード
ord-eae15c7f971b45cc9d743504a091be6d
出典データセット
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03970454

反応ノート

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