Hydrogen iodide → 4-(1-(2-(1H-Imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic Acid Salt

HRID 2230619ノート

反応式

HRID 2230619 の反応式
C(OC([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[N:19]([CH2:20][CH2:21][N:22]3[CH:26]=[CH:25][N:24]=[CH:23]3)[C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=3[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.[IH:31]>CO>[IH:31].[N:22]1([CH2:21][CH2:20][N:19]2[C:18]3[CH:27]=[CH:28][CH:29]=[CH:30][C:17]=3[N:16]=[C:15]2[N:11]2[CH2:12][CH2:13][CH2:14][NH:8][CH2:9][CH2:10]2)[CH:26]=[CH:25][N:24]=[CH:23]1

参加物

4

反応物 2

HCID 24841Hydrogen iodideHCID 184648321-(t-butoxycarbonyl)-4-(1-(2-(1H-imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane

生成物 1

HCID 865838944-(1-(2-(1H-Imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane hydriodic Acid Salt

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Combine 1-(t-butoxycarbonyl)-4-(1-(2-(1H-imidazol-1-yl)ethyl)-1H-benzimidazol-2-yl)[1,4]diazepane (0.22 g, 0.54 mmol), 57% hydriodic acid (0.25 mL, 1.13 mmol), methanol (10 mL) and heat to reflux. After 20 hours, cool the reaction mixture and evaporate in vacuo to give a residue. Triturate the residue with diethyl ether to give a solid. Repeatedly, decant and add diethyl ether before collecting the solid by filtration, rinse with diethyl ether, and dry in vacuo to give the title compound.

後処理

  1. temperaturecool the reaction mixture
  2. customevaporate in vacuo
  3. customto give a residue
  4. customTriturate the residue with diethyl ether
  5. customto give a solid
  6. customRepeatedly, decant
  7. additionadd diethyl ether
  8. custombefore collecting the solid
  9. filtrationby filtration
  10. washrinse with diethyl ether
  11. customdry in vacuo

出典と根拠

ORDレコード
ord-f990a1df29be4ed2a8e78fd83f863066
出典データセット
uspto-grants-2002_07
特許番号
US06423704B1

反応ノート

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