Hydrochloric Acid → 2-((1-Benzyl-piperidin-4-ylamino)-methyl)-phenyl-ammonium dihydrochloride

HRID 239109ノート

反応式

HRID 239109 の反応式
O.O.[Sn](Cl)[Cl:4].[CH2:6]([N:13]1[CH2:18][CH2:17][CH:16]([NH:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[N+:27]([O-])=O)[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.CN(C=O)C.[ClH:35]>C(O)C>[ClH:4].[ClH:35].[CH2:6]([N:13]1[CH2:14][CH2:15][CH:16]([NH:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=2[NH3+:27])[CH2:17][CH2:18]1)[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 61436Stannous chloride dihydrateHCID 48487621-benzyl-N-[(2-nitrophenyl)methyl]piperidin-4-amine

生成物 1

HCID 866864862-((1-Benzyl-piperidin-4-ylamino)-methyl)-phenyl-ammonium dihydrochloride

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

1 g tin (II) chloride-dihydrate was added to 290 mg (1-benzyl-piperidin-4-yl)-(2-nitro-benzyl)-amine in 18 mL ethanol. The reaction was refluxed for 15 min. DMF was added until the reaction was diluted. Then, 5 mL 10 M HCl in ethanol was added, the solvent was removed, 8 mL acetone was added and the mixture was stirred at RT. The precipitate was filtered to give 550 mg of the desired product. Rf: 0.35 (dichlormethane 9: methanol 1: ammonia 0.1), (M+H)+: 296

後処理

  1. temperatureThe reaction was refluxed for 15 min
  2. additionwas diluted
  3. customthe solvent was removed
  4. addition8 mL acetone was added
  5. filtrationThe precipitate was filtered

出典と根拠

ORDレコード
ord-519a4f876a9b40c0a4e4884e2cf34328
出典データセット
uspto-grants-2014_02
特許番号
US08642774B2

反応ノート

読み込み中…