Propargyl bromide → HCID 12534513、化合物

HRID 1075178ノート

反応式

HRID 1075178 の反応式
[K].[CH3:2][S:3][C:4]1[C:9]([F:10])=[CH:8][NH:7][C:6](=[O:11])[N:5]=1.[CH2:12](Br)[C:13]#[CH:14]>CN(C)C=O>[CH2:14]([N:7]1[CH:8]=[C:9]([F:10])[C:4]([S:3][CH3:2])=[N:5][C:6]1=[O:11])[C:13]#[CH:12]

参加物

5

反応物 3

HCID 7842Propargyl bromideHCID 5462222PotassiumHCID 178503576HCID 178503576、化合物

生成物 1

HCID 12534513HCID 12534513、化合物収率 71%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

The potassium salt of 4-methylthio-5-fluoropyrimid-2-one (0.005 mol) and propargyl bromide (0.06 mol) were stirred together in dimethylformamide (20 ml) for 40 hrs at room temperature. The mixture was then filtered; the filtrate evaporated at reduced pressure (1 mm Hg) and the residue extracted with chloroform (60 ml). The chloroform solution was washed with 1 N NaOH, with water, and dried (MgSO4) before evaporation; yield 71%, m.p. 101°-102° C. (ethyl acetate). (Found: C, 48.50; H, 3.62. Calc. for C8H7SN2O: C, 48.48; H, 3.56).

後処理

  1. filtrationThe mixture was then filtered
  2. customthe filtrate evaporated at reduced pressure (1 mm Hg)
  3. extractionthe residue extracted with chloroform (60 ml)
  4. washThe chloroform solution was washed with 1 N NaOH, with water
  5. dry with materialdried (MgSO4)
  6. custombefore evaporation

出典と根拠

ORDレコード
ord-022e3d27b56145c0855722b24b8f3648
出典データセット
uspto-grants-1983_07
特許番号
US04395406

反応ノート

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