Water → 1-[4-Benzyl-(1-piperazinyl)]isoquinoline

HRID 365293노트

반응식

HRID 365293 반응식
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][N:3]=1.[CH2:12]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(N(CC)C(C)C)(C)C.O>CN(C=O)C>[CH2:12]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[CH:4][N:3]=2)[CH2:21][CH2:20]1)[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 759941-BenzylpiperazineHCID 81531DiisopropylethylamineHCID 140539Isoquinoline, 1-chloro-

생성물 1

HCID 224680261-[4-Benzyl-(1-piperazinyl)]isoquinoline수율 40.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A solution of 1-chloroisoquinoline (1.64 g 10 mmol) in dry DMF (5 ml) was added to a stirred solution of 1-benzylpiperazine (1.85 g, 10.5 mmol) and N,N-diisopropylethylamine (2 ml, 1.5 g, 11.5 mmol) in dry DMF (5 ml) under Ar at room temperature. The solution was stirred at room temperature for 17 h. The yellow solution was heated at 110° C. for 7 h, treated with water (100 ml) and extracted with ether (2×50 ml). The extracts were dried (Na2SO4) and concentrated in vacuo. The residue was chromatographed (SiO2 ; ethyl acetate) to give the product (1.233 g).

후처리

  1. temperatureThe yellow solution was heated at 110° C. for 7 h
  2. extractionextracted with ether (2×50 ml)
  3. dry with materialThe extracts were dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed (SiO2 ; ethyl acetate)

출처 및 근거

ORD 기록
ord-83cf8d208096407f9854c5332bf0ae09
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06127357

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