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Pyrrole → HCID 11188835、化合物

HRID 1883471
ノート
印刷プレビュー

反応式

HRID 1883471 の反応式
[CH3:1][O:2][C:3]([C:5]1[N:6]([CH3:13])[CH:7]=[C:8]([N+:10]([O-])=O)[CH:9]=1)=[O:4].N1C=CC=C1.[F:19][C:20]([F:44])([F:43])[C:21]1[CH:26]=[CH:25][C:24]([S:27][CH2:28][CH2:29][O:30][C:31](=O)[O:32]C2C=CC([N+]([O-])=O)=CC=2)=[CH:23][CH:22]=1.CCN(C(C)C)C(C)C.C1C=CC2N(O)N=NC=2C=1>CC(=O)OCC.C(Cl)Cl.CN(C1C=CN=CC=1)C.[Pd].O>[CH3:13][N:6]1[CH:7]=[C:8]([NH:10][C:31]([O:30][CH2:29][CH2:28][S:27][C:24]2[CH:25]=[CH:26][C:21]([C:20]([F:19])([F:44])[F:43])=[CH:22][CH:23]=2)=[O:32])[CH:9]=[C:5]1[C:3]([O:2][CH3:1])=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 8027PyrroleHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2759930Methyl 1-methyl-4-nitro-1H-pyrrole-2-carboxylateHCID 11165106HCID 11165106、化合物

生成物 1

HCID 11188835HCID 11188835、化合物収率 85.42%

試薬・触媒・溶媒 5

HCID 142844-(Dimethylamino)pyridine触媒HCID 23938Palladium触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

After 1-methyl-4-nitropyrrole-2-carboxylic acid methyl ester (1.17 g, 6.35 mmol) was dissolved in EA (20 ml), 10% Pd/C (50 mg, catalytic weight) was added thereto. The mixture was stirred for 1 hour at room temperature under hydrogen atmosphere to reduce a nitro group (NO2) into an amino group (NH2), whereby a pyrrole-type amino acid was obtained. 10% Pd/C was filtered out by celite 545 filter, and the filtrate was washed with EA and MeOH and concentrated under vacuum. To the residue were added carbonic acid 4-nitro-phenyl ester 2-(4-trifluoromethyl-phenylsulfanyl)-ethyl ester (2.23 g, 5.76 mmol) dissolved in anhydrous DCM (30 ml), DIEA (2.01 μm, 11.56 mmol), DMAP (1.41 g, 11.56 mmol), and HOBt (1.77 g, 11.56 mmol), and the mixture was stirred for 12 hours at room temperature. The reaction was stopped by adding water and the reaction mixture was extracted with DCM. The organic layer was dried over anhydrous MgSO4 and concentrated. The residue was purified by silica gel column chromatography (EA/n-hexane=1/3, v/v) to give methyl 1-methyl-4-[2-(4-trifluoromethyl-phenylsulfanyl)-ethoxycarbonylamino]-1H-pyrrole-2-carboxylate (1.98 g, 85.42%) of a pale yellow solid.

後処理

  1. customwas obtained
  2. filtration10% Pd/C was filtered out by celite 545
  3. filtrationfilter
  4. washthe filtrate was washed with EA and MeOH
  5. concentrationconcentrated under vacuum
  6. extractionthe reaction mixture was extracted with DCM
  7. dry with materialThe organic layer was dried over anhydrous MgSO4
  8. concentrationconcentrated
  9. customThe residue was purified by silica gel column chromatography (EA/n-hexane=1/3

出典と根拠

ORDレコード
ord-9ec5679d050247aaafdbd1d23056dd5e
出典データセット
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06759511B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート