Ethanol → 2-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-5-(3-pyridyl)methyl-4-pyrimidone

HRID 358460ノート

反応式

HRID 358460 の反応式
[N+]([NH:4][C:5]1[NH:10][C:9](=[O:11])[C:8]([CH2:12][C:13]2[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=2)=[CH:7][N:6]=1)([O-])=O.[CH3:19][N:20]([CH2:22][C:23]1[S:24][CH:25]=[C:26]([CH2:28][S:29][CH2:30][CH2:31]N)[N:27]=1)[CH3:21].C(O)C>O>[CH3:21][N:20]([CH2:22][C:23]1[S:24][CH:25]=[C:26]([CH2:28][S:29][CH2:30][CH2:31][NH:4][C:5]2[NH:10][C:9](=[O:11])[C:8]([CH2:12][C:13]3[CH:14]=[N:15][CH:16]=[CH:17][CH:18]=3)=[CH:7][N:6]=2)[N:27]=1)[CH3:19]

参加物

5

反応物 3

HCID 702EthanolHCID 109773182-(Dimethylaminomethyl)-4-(2-aminoethylthiomethyl)thiazoleHCID 12788688N-{6-Oxo-5-[(pyridin-3-yl)methyl]-1,6-dihydropyrimidin-2-yl}nitramide

生成物 1

HCID 133734772-[2-(2-Dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-5-(3-pyridyl)methyl-4-pyrimidone

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A reaction mixture prepared from 1.24 g. of 2-nitroamino-5-(3-pyridyl)methyl-4-pyrimidone, 1.14 g. of 2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethylamine and 6 ml. of anhydrous ethanol was refluxed for about 1 day under a nitrogen atmosphere. The volatile constitutents were removed by evaporation to yield an oily residue. Water was added and the aqueous layer extracted with ether and with ethyl acetate. The organic extracts were combined, dried and evaporated to dryness to yield 2-[2-(2-dimethylaminomethyl-4-thiazolylmethylthio)ethyl]amino-5-(3-pyridyl)methyl-4-pyrimidone as a residue which was crystallized from ether. Recrystallization from an ethanol-ether solvent mixture yielded 2-[2-(2-dimethylaminomethyle-4-thiazolylmethylthio)ethyl]amino-5-(3-pyridyl)methyl-4-pyrimidone melting at 122°-123° C.; yield=0.68 g.

後処理

  1. customA reaction mixture prepared from 1.24 g
  2. customThe volatile constitutents were removed by evaporation
  3. customto yield an oily residue
  4. extractionthe aqueous layer extracted with ether and with ethyl acetate
  5. customdried
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-d2e4b20cefc24253b89817d5bff47df1
出典データセット
uspto-grants-1984_08
特許番号
US04468399

反応ノート

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