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Chlorosuccinimide → HCID 178494681、化合物

HRID 1488113
ノート
印刷プレビュー

反応式

HRID 1488113 の反応式
[CH3:1][O:2][CH2:3][C:4]1[NH:5][C:6]([C:9]2[C:10]([CH3:20])=[CH:11][C:12]([CH3:19])=[C:13]([CH:18]=2)[C:14]([O:16][CH3:17])=[O:15])=[CH:7][N:8]=1.C1C(=O)N([Cl:28])C(=O)C1>C(Cl)(Cl)Cl>[Cl:28][C:7]1[N:8]=[C:4]([CH2:3][O:2][CH3:1])[NH:5][C:6]=1[C:9]1[C:10]([CH3:20])=[CH:11][C:12]([CH3:19])=[C:13]([CH:18]=1)[C:14]([O:16][CH3:17])=[O:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 90033625Methyl 5-(2-(methoxymethyl)-1H-imidazol-5-yl)-2,4-dimethylbenzoate2 回

生成物 1

HCID 178494681HCID 178494681、化合物収率 38%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Into a 100-mL round-bottom flask, was placed a solution of methyl 5-(2-(methoxymethyl)-1H-imidazol-5-yl)-2,4-dimethylbenzoate (compound 230.5, 70 mg, 0.26 mmol) in chloroform (6 mL). NCS (35 mg, 0.26 mmol) was added to the reaction. The reaction mixture was stirred overnight at room temperature, then quenched with 1 mL of water. The aqueous phase was extracted with 2×5 mL of dichloromethane and the combined organic layers were concentrated under reduced pressure. The residue was applied onto a silica gel chromatography with ethyl acetate/petroleum ether (1:10) as eluent to yield 30 mg (38%) of the title compound as a white crude solid.

後処理

  1. customInto a 100-mL round-bottom flask, was placed
  2. customquenched with 1 mL of water
  3. extractionThe aqueous phase was extracted with 2×5 mL of dichloromethane
  4. concentrationthe combined organic layers were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f4e0c7368fda432583ebebe69f4f668b
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428502B2

反応ノート

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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