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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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Methyl chloroglyoxylate → HCID 58504269、化合物

HRID 2407786
ノート
印刷プレビュー

反応式

HRID 2407786 の反応式
[CH3:1][O:2][CH:3]([O:34][CH3:35])[CH2:4][NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12](=[O:33])[CH2:13][CH2:14][CH:15]1[CH2:20][CH2:19][N:18]([CH2:21][C:22]2[S:26][C:25]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=3)=[N:24][CH:23]=2)[CH2:17][CH2:16]1.C(N(C(C)C)CC)(C)C.Cl[C:46](=[O:51])[C:47]([O:49][CH3:50])=[O:48]>ClCCl.C(OCC)(=O)C>[CH3:35][O:34][CH:3]([O:2][CH3:1])[CH2:4][N:5]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12](=[O:33])[CH2:13][CH2:14][CH:15]1[CH2:20][CH2:19][N:18]([CH2:21][C:22]2[S:26][C:25]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=3)=[N:24][CH:23]=2)[CH2:17][CH2:16]1)[C:46](=[O:51])[C:47]([O:49][CH3:50])=[O:48]
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 79846Methyl chloroglyoxylateHCID 81531DiisopropylethylamineHCID 58504215HCID 58504215、化合物

生成物 1

HCID 58504269HCID 58504269、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of the compound prepared in Example 323 (555 mg) in dichloromethane (7.0 mL) at 0° C. was added diisopropylethylamine (0.59 mL) followed by methyl 2-chloro-2-oxoacetate (0.16 mL). The reaction was allowed to warm to room temperature and then stirred for 2 hours. The solution was diluted with ethyl acetate, washed with saturated aqueous sodium bicarbonate solution and brine. The organics were dried over magnesium sulfate, filtered and concentrated under reduced pressure to afford the crude material, which was purified by flash column chromatography (eluant: 80% ethyl acetate/hexane with 3% (9:1 methanol/concentrated ammonium hydroxide)) to furnish the title compound (392 mg) with the following physical properties.

後処理

  1. washwashed with saturated aqueous sodium bicarbonate solution and brine
  2. dry with materialThe organics were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customto afford the crude material, which
  6. customwas purified by flash column chromatography (eluant: 80% ethyl acetate/hexane with 3% (9:1 methanol/concentrated ammonium hydroxide))

出典と根拠

ORDレコード
ord-532bfe765c4c4de1a5f12a8759c4fa1c
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809538B2

反応ノート

読み込み中…

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