Dimethylformamide → 1,3-dihydro-1,3-dioxo-2H-isoindole-2-propionyl chloride

HRID 520305ノート

反応式

HRID 520305 の反応式
[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH2:12][CH2:13][C:14]([OH:16])=O.C(Cl)(=O)C([Cl:20])=O.CN(C=O)C>C(Cl)Cl>[O:1]=[C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[N:3]1[CH2:12][CH2:13][C:14]([Cl:20])=[O:16]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 768593-Phthalimidopropionic acid

生成物 1

HCID 869661,3-dihydro-1,3-dioxo-2H-isoindole-2-propionyl chloride収率 92.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 137g (20.0 g, 91 mmol) in DCM (250 mL) were added oxalyl chloride (13.8 g, 109 mmol) and DMF (0.1 mL). See FIG. 2. The mixture was stirred at RT for 4 h. Upon reaction completion, the mixture was concentrated to give 3-(1,3-dioxoisoindolin-2-yl)propanoyl chloride 137h (20.0 g, 92%) as a white solid.

後処理

  1. customUpon reaction completion
  2. concentrationthe mixture was concentrated

出典と根拠

ORDレコード
ord-b6900d05179d4d31bae4a8dc6a913546
出典データセット
uspto-grants-2016_05
特許番号
US09326985B2

反応ノート

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