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Triphenylarsine → 5-isoquinolin-4-yl-1H-pyrrole-2-carboxylic acid methyl ester

HRID 985611
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반응식

HRID 985611 반응식
[CH3:1][O:2][C:3]([C:5]1[NH:6][C:7](Br)=[CH:8][CH:9]=1)=[O:4].C1([As](C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C[Sn](C)(C)[C:32]1[C:41]2[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=2)[CH:35]=[N:34][CH:33]=1>CN1C(=O)CCC1.[Pd].[Pd].C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1.C(=CC(C=CC1C=CC=CC=1)=O)C1C=CC=CC=1>[CH3:1][O:2][C:3]([C:5]1[NH:6][C:7]([C:32]2[C:41]3[C:36](=[CH:37][CH:38]=[CH:39][CH:40]=3)[CH:35]=[N:34][CH:33]=2)=[CH:8][CH:9]=1)=[O:4]
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참가 물질

6

반응물 3

HCID 11773TriphenylarsineHCID 11600885Methyl 5-bromo-1H-pyrrole-2-carboxylateHCID 127591074-(Trimethylstannyl)isoquinoline

생성물 1

HCID 697453555-isoquinolin-4-yl-1H-pyrrole-2-carboxylic acid methyl ester수율 55%

시약·촉매·용매 2

HCID 9832798Tris(dibenzylideneacetone) dipalladium
촉매
HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

5-Bromo-1H-pyrrole-2-carboxylic acid methyl ester (1.49 mmol, 0.30 g, prepared according to the procedure described in Method 4 of Example 2) in NMP (10 ml) was treated with triphenylarsine (0.30 mmol, 91 mg), tris(dibenzylideneacetone) dipalladium(0) (0.07 mmol, 68 mg), and 4-(trimethylstannyl)-isoquinoline (2.22 mmol, 0.65 g), then heated to reflux under an argon atmosphere overnight. The resulting mixture was concentrated under reduced pressure, then purified by silica gel chromatography to provide 0.21 g (55%) of 5-isoquinolin-4-yl-1H-pyrrole-2-carboxylic acid methyl ester. 1H NMR (CDCl3) δ 9.81 (1H, br s), 9.35 (1H, s), 8.66 (1H, s), 8.31 (1H, d, J=8.5), 8.10 (1H, d, J=8.1), 7.91 (1H, t, J=15.2), 7.79 (1H, t, J=15.2), 7.11 (1H, dd, J=3.8, 2.5), 6.64 (1H, dd, J=3.7, 2.7), 3.90 (3H, s).

후처리

  1. temperatureheated
  2. temperatureto reflux under an argon atmosphere overnight
  3. concentrationThe resulting mixture was concentrated under reduced pressure
  4. custompurified by silica gel chromatography

출처 및 근거

ORD 기록
ord-fd6a3cbfe1a74ea69f5591526f29e6e9
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06872745B2

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