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Triethylamine → 1-(4-Nitro-1-oxoisoindolin-2-yl)propane-1,3-dicarboxylic acid dibenzyl ester

HRID 844226
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HRID 844226 반응식
[N+:1]([C:4]1[C:5]([CH2:14]Br)=[C:6]([CH:11]=[CH:12][CH:13]=1)[C:7]([O:9]C)=O)([O-:3])=[O:2].C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH2:27]([O:34][C:35](=[O:50])[C@H:36]([CH2:38][CH2:39][C:40]([O:42][CH2:43][C:44]1[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1)=[O:41])[NH2:37])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1.C(N(CC)CC)C>C1COCC1.C(Cl)Cl>[CH2:27]([O:34][C:35]([CH:36]([N:37]1[CH2:14][C:5]2[C:6](=[CH:11][CH:12]=[CH:13][C:4]=2[N+:1]([O-:3])=[O:2])[C:7]1=[O:9])[CH2:38][CH2:39][C:40]([O:42][CH2:43][C:44]1[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1)=[O:41])=[O:50])[C:28]1[CH:29]=[CH:30][CH:31]=[CH:32][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 1487795Methyl 2-(bromomethyl)-3-nitrobenzoateHCID 13233366L-Glutamic acid dibenzyl ester tosylate

생성물 1

HCID 155498421-(4-Nitro-1-oxoisoindolin-2-yl)propane-1,3-dicarboxylic acid dibenzyl ester수율 59.5%

시약·촉매·용매 2

HCID 6344Dichloromethane용매
HCID 8028
Tetrahydrofuran
용매

실험 절차

A mixture of methyl 3-nitro-2-(bromomethyl)benzoate (2.5 g, 9.12 mmol), L-glutamic acid dibenzyl ester p-toluenesulfonate salt (3.0 g, 9.12 mmol) and triethylamine (2.0 g, 20.0 mmol) in THF (50 mL) is heated at reflux for 16 hours. The mixture is diluted with methylene chloride (150 mL) and washed with water (2×40 mL), brine (40 mL), dried and concentrated to an oil. The oil is purified by chromatography (silica gel, Hexane:ethoxyacetic acid 7:3) to give 1-(4-nitro-1-oxoisoindolin-2-yl)propane-1,3-dicarboxylic acid dibenzyl ester (2.65 g, 59%); 1H NMR (CDCl3) δ8.39 (d, J=7.8 Hz, 1H), 8.16 (d, J=7.3 Hz, 1H), 7.69 (t, J=7.9 Hz, 1H), 7.30 (m, 10H), 5.29 (s, 2H), 5.29-5.13 (m, 1H), 5.03 (s, 2H), 4.98 (d, J=19.1 Hz, 1H), 4.85 (d, J=19.2 Hz, 1H), 2.54-2.39 (m, 4H); 13C NMR (CDCl3) δ171.79, 169.92, 166.72, 143.47, 137.25, 135.49, 135.04, 134.99, 130.17, 129.67, 128.62, 128.52, 128.29, 128.25, 128.23, 127.04, 67.49, 66.58, 53.70, 48.35, 30.87, 24.79.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 16 hours
  3. washwashed with water (2×40 mL), brine (40 mL)
  4. customdried
  5. concentrationconcentrated to an oil
  6. customThe oil is purified by chromatography (silica gel, Hexane:ethoxyacetic acid 7:3)

출처 및 근거

ORD 기록
ord-420a4f4a15cc4e03ad53b427e95fe004
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06380239B1

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