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Sodium methanethiolate → 6,7-Dichloro-2, 3-dimethoxy-5-methylthiomethylquinoxaline

HRID 1458594
ノート
印刷プレビュー

反応式

HRID 1458594 の反応式
[CH3:1][S-:2].[Na+].Br[CH2:5][C:6]1[C:15]([Cl:16])=[C:14]([Cl:17])[CH:13]=[C:12]2[C:7]=1[N:8]=[C:9]([O:20][CH3:21])[C:10]([O:18][CH3:19])=[N:11]2>CN(C)C=O>[Cl:16][C:15]1[C:6]([CH2:5][S:2][CH3:1])=[C:7]2[C:12](=[CH:13][C:14]=1[Cl:17])[N:11]=[C:10]([O:18][CH3:19])[C:9]([O:20][CH3:21])=[N:8]2
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 4378561Sodium methanethiolateHCID 105459165-Bromomethyl-6,7-dichloro-2,3-dimethoxyquinoxaline

生成物 1

HCID 220970456,7-Dichloro-2, 3-dimethoxy-5-methylthiomethylquinoxaline収率 87.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Sodium methanethiolate (22 mg, 0.312 mmol) was added to a stirred solution of 5-bromomethyl-6,7-dichloro-2,3-dimethoxyquinoxaline (see Preparation 28) (100 mg, 0.284 mmol) in dry dimethylformamide (5 ml) under nitrogen at room temperature. The mixture was stirred for 10 minutes and was then quenched with brine and extracted twice with dichloromethane. The combined extracts were dried (MgSO4) and concentrated under reduced pressure. The residue was purified by flash chromatography (eluting with 1:1 hexane:dichloromethane) to give 6,7-dichloro-2, 3-dimethoxy-5-methylthiomethylquinoxaline (79 mg, 87%) as a white solid, m.p. 143°-5° C.

後処理

  1. customwas then quenched with brine
  2. extractionextracted twice with dichloromethane
  3. dry with materialThe combined extracts were dried (MgSO4)
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by flash chromatography (eluting with 1:1 hexane:dichloromethane)

出典と根拠

ORDレコード
ord-639e21361ad645be97e0ac43b18e9563
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05852016

反応ノート

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