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Sodium Carbonate → HCID 73426448、化合物

HRID 1507558
ノート
印刷プレビュー

反応式

HRID 1507558 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]([OH:9])=O.[NH2:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([CH3:23])([CH3:22])[C:16](=[O:21])[N:17]2[CH3:20])=[CH:13][CH:12]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C.C(OCC)(=O)C>[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[C:7]([NH:10][C:11]1[CH:19]=[C:18]2[C:14]([C:15]([CH3:23])([CH3:22])[C:16](=[O:21])[N:17]2[CH3:20])=[CH:13][CH:12]=1)=[O:9]
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 5

HCID 10340Sodium CarbonateHCID 81531DiisopropylethylamineHCID 5576781-methyl-1H-imidazole-2-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 529112486-Amino-1,3,3-trimethyl-1,3-dihydro-2H-indol-2-one

生成物 1

HCID 73426448
HCID 73426448、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-methyl-1H-imidazole-2-carboxylic acid (99.4 mg, 788 μmol) and 6-amino-1,3,3-trimethylindolin-2-one (100 mg, 526 μmol) in DMF (3 ml) were added HATU (400 mg, 1.05 mmol) and DIPEA (347 mg, 468 μl, 2.63 mmol). The reaction mixture was stirred for 3 hours at room temperature and then poured into ethyl acetate and 1 M aqueous sodium carbonate solution. The aqueous phase was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and the solvent was removed under reduced pressure. The crude material was purified by silica gel chromatography using ethyl acetate/heptane as eluent followed by reversed phase preparative HPLC. The title compound was obtained as off-white crystals (135 mg).

後処理

  1. extractionThe aqueous phase was extracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. customthe solvent was removed under reduced pressure
  4. customThe crude material was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-ae0a3ff2b1c24a64a750c29710c90868
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09221816B2

反応ノート

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