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Diisopropylamine → 4-[4-(5-Bromo-1-oxo-1,2-dihydro-isoquinolin-3-yl)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester

HRID 717081
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HRID 717081 반응식
C(NC(C)C)(C)C.[Li]CCCC.[Br:13][C:14]1[C:15]([CH3:27])=[C:16]([CH:24]=[CH:25][CH:26]=1)[C:17]([N:19]([CH2:22][CH3:23])CC)=[O:18].[C:28]([O:32][C:33]([N:35]1[CH2:40][CH2:39][N:38]([CH2:41][C:42]2[CH:47]=[CH:46]C(C#N)=[CH:44][CH:43]=2)[CH2:37][CH2:36]1)=[O:34])([CH3:31])([CH3:30])[CH3:29]>C1COCC1>[C:28]([O:32][C:33]([N:35]1[CH2:40][CH2:39][N:38]([CH2:41][C:42]2[CH:47]=[CH:46][C:23]([C:22]3[NH:19][C:17](=[O:18])[C:16]4[C:15]([CH:27]=3)=[C:14]([Br:13])[CH:26]=[CH:25][CH:24]=4)=[CH:44][CH:43]=2)[CH2:37][CH2:36]1)=[O:34])([CH3:31])([CH3:30])[CH3:29]
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참가 물질

6

반응물 4

HCID 7912DiisopropylamineHCID 183822571-Boc-4-(4-Cyanobenzyl)piperazineHCID 655438803-bromo-N,N-diethyl-2-methyl-benzamideHCID 178418339Butyllithium

생성물 1

HCID 717351534-[4-(5-Bromo-1-oxo-1,2-dihydro-isoquinolin-3-yl)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester수율 66.2%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

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온도
-78 °C

실험 절차

To a stirred solution of N,N-diisopropylamine (1.56 mL, 11.10 mmol) in THF (5 mL) under N2 at −78° C. was added n-BuLi (2.5M in hexanes) (4.44 mL, 11.10 mmol) and the reaction stirred at −78° C. for 20 min, after which time a solution of 3-bromo-N,N-diethyl-2-methyl-benzamide (1 g, 3.70 mmol) in THF (5 mL) was added, and the reaction stirred at −78° C. for 30 minutes. A solution of 4-(4-cyano-benzyl)-piperazine-1-carboxylic acid tert-butyl ester (1.15 g, 3.70 mmol) in THF (5 mL) was added and the reaction stirred at −78° C. for 2 h. The reaction was quenched with ice and water, EtOAc added and concentrated in vacuo. The crude material was purified by silica gel column chromatography, eluting with isohexane and increasing the polarity to 100% EtOAc to afford 4-[4-(5-bromo-1-oxo-1,2-dihydro-isoquinolin-3-yl)-benzyl]-piperazine-1-carboxylic acid tert-butyl ester as a cream solid (1.22 g, 66%).

후처리

  1. stirringthe reaction stirred at −78° C. for 30 minutes
  2. stirringthe reaction stirred at −78° C. for 2 h
  3. customThe reaction was quenched with ice and water, EtOAc
  4. additionadded
  5. concentrationconcentrated in vacuo
  6. customThe crude material was purified by silica gel column chromatography
  7. washeluting with isohexane
  8. temperatureincreasing the polarity to 100% EtOAc

출처 및 근거

ORD 기록
ord-a8caf5504b0a463abffcb360a16ff69a
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09193689B2

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