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

반응식

HRID 324485 반응식
[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

참가 물질

4

반응물 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

생성물 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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d5bc3205c97433d978de526e17fa292
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06218376B1

연결된 노트

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