Trimethyl orthovalerate → 2-butyl-1H-thieno[3,4-d]imidazole

HRID 248380

反応式

HRID 248380 の反応式
[NH2:1][C:2]1[C:6]([NH2:7])=[CH:5][S:4][CH:3]=1.[C:8](OC)(OC)(OC)[CH2:9][CH2:10][CH2:11][CH3:12].C1(C)C=CC(S([O-])(=O)=O)=CC=1.[NH+]1C=CC=CC=1>C(O)C>[CH2:9]([C:8]1[NH:1][C:2]2=[CH:3][S:4][CH:5]=[C:6]2[N:7]=1)[CH2:10][CH2:11][CH3:12]

参加物

5

反応物 3

HCID 83755Trimethyl orthovalerateHCID 466102Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1)HCID 643216Thiophene-3,4-diamine

生成物 1

HCID 193706342-butyl-1H-thieno[3,4-d]imidazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 3,4-diaminothiophene (156 mg) in ethanol (10 ml) was added trimethyl orthovalerate (0.29 ml) and pyridinium p-toluenesulfonate (4 mg). The mixture was refluxed for one hour and concentrated in vacuo. The residue was purified by preparative thin layer chromatography on silica gel developed by ethyl acetate to give 2-butyl-1H-thieno[3,4-d]imidazole (155 mg) as crystals.

後処理

  1. temperatureThe mixture was refluxed for one hour
  2. concentrationconcentrated in vacuo
  3. customThe residue was purified by preparative thin layer chromatography on silica gel

出典と根拠

ORDレコード
ord-354f919044724ce2b749849551db4a26
出典データセット
uspto-grants-1993_05
特許番号
US05210092

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