Potassium Carbonate → HCID 22099464, 화합물

HRID 1457605노트

반응식

HRID 1457605 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 22099464HCID 22099464, 화합물수율 70.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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-).

후처리

  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)

출처 및 근거

ORD 기록
ord-8882b3d22c5349a2adaff0d47fe1a0e0
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849732

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