Phosphorus sulfide (P2S5) → (+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-3,4-dihydro-4-thioxo-2(1H)-pyrimidinone

HRID 324485

反応式

HRID 324485 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:16]([C:17]3[C:18](=O)[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:10]3[N:11]=[C:12]([CH3:15])[N:13]([CH3:14])[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:26]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:28]>O1CCOCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[CH:16]([C:17]3[C:18](=[S:28])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:10]3[N:11]=[C:12]([CH3:15])[N:13]([CH3:14])[C:9]=3[CH:8]=[CH:7][C:6]=2[CH:26]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 22003604(+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

生成物 1

HCID 9864902(+/-)-5-(7-Chloro-1,2-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]imidazol-4-yl)-1-methyl-3,4-dihydro-4-thioxo-2(1H)-pyrimidinone

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

A mixture of the product from step (iv) (0.535 g), and phosphorus pentasulphide (0.967 g) in 1,4-dioxane (10 ml) was heated at 100° C. for 3 h. The solvent evaporated and the residue dissolved in dichloromethane, washed with saturated aqueous sodium bicarbonate solution then with water, dried (MgSO4) and evaporated. Purification was by chromatography on a biotage silica column, using 3% methanol/0.1% 0.880 ammonia in dichloromethane as eluant.

後処理

  1. customThe solvent evaporated
  2. dissolutionthe residue dissolved in dichloromethane
  3. washwashed with saturated aqueous sodium bicarbonate solution
  4. dry with materialwith water, dried (MgSO4)
  5. customevaporated
  6. customPurification

出典と根拠

ORDレコード
ord-8d5bc3205c97433d978de526e17fa292
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

関連ノート

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