Potassium Carbonate → HCID 22099464、化合物

HRID 1457605ノート

反応式

HRID 1457605 の反応式
[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13]I)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:15]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)P(N(C)C)(N(C)C)=O>O>[CH2:1]([O:8][C:9]([NH:11][CH2:12][CH2:13][N:25]1[CH2:26][CH2:27][N:22]([CH2:15][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH2:23][CH2:24]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 12679HexamethylphosphoramideHCID 759941-BenzylpiperazineHCID 11301181Benzyl (2-iodoethyl)carbamate

生成物 1

HCID 22099464HCID 22099464、化合物収率 70.2%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 6.92 g of N-benzyloxycarbonyl-2-iodo-ethylamine, 4.00 g of 1-benzylpiperazine, 15.66 g of potassium carbonate and 40 ml of hexamethylphosphoramide (HMPA) was stirred at room temperature for overnight. Water was added to the reaction mixture, and the resulting mixture was extracted with diethyl ether. The extract was washed and dried, and the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (solvent; chloroform:methanol=15:1) to give 5.63 g of N-benzyloxycarbonyl-2-(4-benzylpiperazin-1-yl)ethylamine (yield: 70%, oily product, IR: 3230, 2910, 1710 cm-).

後処理

  1. extractionthe resulting mixture was extracted with diethyl ether
  2. washThe extract was washed
  3. customdried
  4. customthe solvent was removed under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (solvent; chloroform:methanol=15:1)

出典と根拠

ORDレコード
ord-8882b3d22c5349a2adaff0d47fe1a0e0
出典データセット
uspto-grants-1998_12
特許番号
US05849732

反応ノート

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