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Diisopropylethylamine → HCID 71730367、化合物

HRID 1056205
ノート
印刷プレビュー

反応式

HRID 1056205 の反応式
C([NH:5]C1C(C)=NC2C(N=1)=C(C1NC3CN[C:23](=[O:24])C=3C=1)C=CC=2)(C)(C)C.Cl.[NH2:27][CH2:28][C:29]1[NH:30][C:31]([C:37]2[CH:46]=[CH:45][CH:44]=[C:43]3[C:38]=2[N:39]=[C:40]([NH:48][C:49]([CH3:52])([CH3:51])[CH3:50])[C:41]([CH3:47])=[N:42]3)=[CH:32][C:33]=1[C:34]([OH:36])=O.CCN(C(C)C)C(C)C.F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1>C(Cl)Cl.CN(C=O)C>[NH3:5].[CH3:23][OH:24].[C:49]([NH:48][C:40]1[C:41]([CH3:47])=[N:42][C:43]2[C:38]([N:39]=1)=[C:37]([C:31]1[NH:30][C:29]3[CH2:28][NH:27][C:34](=[O:36])[C:33]=3[CH:32]=1)[CH:46]=[CH:45][CH:44]=2)([CH3:52])([CH3:51])[CH3:50]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 71730367HCID 71730367、化合物HCID 89783476HCID 89783476、化合物

生成物 2

HCID 21705897Ammonia methanol収率 0%HCID 71730367HCID 71730367、化合物収率 52%

試薬・触媒・溶媒

2
HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

Preparation 2-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (334). To a 100-mL round-bottomed flask was added 2-(aminomethyl)-5-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-1H-pyrrole-3-carboxylic acid hydrochloride (334c) (0.21 g, 0.55 mmol), DCM (10 mL), DMF (10 mL), DIEA (0.29 mL, 1.65 mmol), and (benzotriazol-1-yloxy)tripyrrolidinophosphonium hexafluorophosphate (0.34 g, 0.66 mmol) (Sigma-Aldrich Chemical Company, Inc.). The reaction mixture was stirred at RT for 30 min, concentrated to half of its volume, and diluted with EtOAc (10 mL). The organic extract was washed with sat NaHCO3 (5 mL), dried over Na2SO4, and concentrated. The crude material was absorbed onto a plug of silica gel and purified by chromatography through a Redi-Sep pre-packed silica gel column (12 g), eluted first with 30% EtOAc in hexanes, and then with a gradient of 0-4% 2 M NH3/MeOH in DCM to provide 2-(3-(tert-butylamino)-2-methylquinoxalin-5-yl)-5,6-dihydropyrrolo[3,4-b]pyrrol-4(1H)-one (334) (97 mg, 52% yield) as a yellow solid. 1H NMR (400 MHz, DMSO-d6) δ 12.08 (br. s., 1H), 7.82 (d, J=7.24 Hz, 1H), 7.63 (d, J=8.02 Hz, 1H), 7.53 (s, 1H), 7.37 (t, J=7.73 Hz, 1H), 6.94 (s, 1H), 6.02 (s, 1H), 4.29 (s, 2H), 2.58 (s, 3H), 1.55 (s, 9H). m/z (ESI, +ve) 336.2 (M+H)+.

後処理

  1. concentrationconcentrated to half of its volume
  2. additiondiluted with EtOAc (10 mL)
  3. extractionThe organic extract
  4. washwas washed with sat NaHCO3 (5 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated
  7. customThe crude material was absorbed onto a plug of silica gel
  8. custompurified by chromatography through a Redi-Sep pre-packed silica gel column (12 g)
  9. washeluted first with 30% EtOAc in hexanes

出典と根拠

ORDレコード
ord-db01a97807e9474896c5d9db4f1306b9
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394297B2

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