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Hexane → Methyl 2-[(3-oxo-1,2,3,4-tetrahydroquinoxalin-6-yl)carbonyl]benzoate

HRID 2367090
ノート
印刷プレビュー

反応式

HRID 2367090 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]([C:22]([C:24]2[CH:39]=[CH:38][CH:37]=[CH:36][C:25]=2[C:26]([O:28][CH2:29]C2C=CC=CC=2)=[O:27])=[O:23])[CH:7]=[CH:8][C:9]=1[NH:10][CH2:11][C:12](=[O:21])OCC1C=CC=CC=1)([O-])=O.C[Si](C=[N+]=[N-])(C)C.CCCCCC>O1CCCC1.C(OCC)(=O)C.C1(CO)C=CC=CC=1>[O:21]=[C:12]1[NH:1][C:4]2[C:9](=[CH:8][CH:7]=[C:6]([C:22]([C:24]3[CH:39]=[CH:38][CH:37]=[CH:36][C:25]=3[C:26]([O:28][CH3:29])=[O:27])=[O:23])[CH:5]=2)[NH:10][CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8058HexaneHCID 167693TrimethylsilyldiazomethaneHCID 67045250Phenylmethyl 2-{[3-nitro-4-({2-oxo-2-[(phenylmethyl)oxy]ethyl}amino)phenyl]carbonyl}benzoate

生成物 1

HCID 67044874Methyl 2-[(3-oxo-1,2,3,4-tetrahydroquinoxalin-6-yl)carbonyl]benzoate収率 67%

試薬・触媒・溶媒 2

HCID 244Benzyl Alcohol溶媒
HCID 21939870
Tetrahydrofuran ethyl acetate
溶媒

実験手順

A solution of phenylmethyl 2-{[3-nitro-4-({2-oxo-2-[(phenylmethyl)oxy]ethyl}amino)phenyl]carbonyl}benzoate (0.31 g, 0.59 mmol) in a mixture of tetrahydrofurane-ethyl acetate (1:1, 50 mL) was hydrogenated in the presence of 10% Pd/C (0.15 g) in a Parr shaker at 40 psi, until the consumption of hydrogen ceased. The catalyst was filtered off and the solvent was evaporated. The resulting crude product was converted into its methyl ester in a mixture of benzene-methanol (9:1, 5.0 mL) by the addition of 2.0 M trimethylsilyldiazomethane solution in hexane (0.3 mL, 0.60 mmol). The reaction was quenched by the addition of a few drops of acetic acid and the solvent was evaporated. The resulting crude product was purified by silica gel flash chromatography (hexane:ethyl acetate 4:1 to 1:1 eluent) to give methyl 2-[(3-oxo-1,2,3,4-tetrahydroquinoxalin-6-yl)carbonyl]benzoate (0.12 g, 67% yield). 1H NMR (400 MHz, DMSO-d6): 8.06 (s, 1H), 7.83 (dd, 1H), 7.64 (d, 1H), 7.52 (t, 1H), 7.38 (d, 1H), 7.09 (7.03 (d, 1H), 4.41 (s, 2H), 3.77 (s, 3H); MS (EI) for C17H14N2O4: 311 (MH+).

後処理

  1. customwas hydrogenated in the presence of 10% Pd/C (0.15 g) in a Parr shaker at 40 psi, until the consumption of hydrogen
  2. filtrationThe catalyst was filtered off
  3. customthe solvent was evaporated
  4. customThe reaction was quenched by the addition of a few drops of acetic acid
  5. customthe solvent was evaporated
  6. customThe resulting crude product was purified by silica gel flash chromatography (hexane:ethyl acetate 4:1 to 1:1 eluent)

出典と根拠

ORDレコード
ord-4d1166e7edf842e6b1b9a3d3e1174b98
出典データセット
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08697737B2

反応ノート

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