Sulfuric Acid → 2-Chloro-3-(2-oxopyrrolidin-1-yl)propanal

HRID 1896387

反応式

HRID 1896387 の反応式
O[CH2:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[O:8].S(=O)(=O)(O)O.[Cl:14][CH:15]=[CH:16]Cl.C([O-])([O-])=[O:19].[K+].[K+]>O>[Cl:14][CH:15]([CH2:2][N:3]1[CH2:7][CH2:6][CH2:5][C:4]1=[O:8])[CH:16]=[O:19]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 109001,2-DichloroethyleneHCID 11430Potassium CarbonateHCID 849112-Pyrrolidinone, 1-(hydroxymethyl)-

生成物 1

HCID 536291632-Chloro-3-(2-oxopyrrolidin-1-yl)propanal

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
40 °C

実験手順

In a 250 ml, three-necked flask fitted with a magnetic stirrer, 1-(hydroxymethyl)pyrrolidin-2-one x82 (15 g, 0.13 mol) is cooled to −10° C. Cold concentrated sulfuric acid (150 ml) is added dropwise. At this temperature, 1,2-dichloroethene (46.73 g, 0.482 mol) is added while the temperature is kept below 0° C. At the end of the addition the mixture is stirred at 40° C. for 2 h. Water is added and the pH is adjusted with K2CO3. The aqueous phase is extracted with CH2Cl2, the combined organic phases are dried over MgSO4, filtered and concentrated. The crude 2-chloro-3-(2-oxopyrrolidin-1-yl)propanal x83 is used in the next step without any further purification.

後処理

  1. customIn a 250 ml, three-necked flask fitted with a magnetic stirrer
  2. customis kept below 0° C
  3. additionAt the end of the addition the mixture
  4. extractionThe aqueous phase is extracted with CH2Cl2
  5. dry with materialthe combined organic phases are dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe crude 2-chloro-3-(2-oxopyrrolidin-1-yl)propanal x83 is used in the next step without any further purification

出典と根拠

ORDレコード
ord-bb9515b5a4394681a0b7360f5cfcf5e3
出典データセット
uspto-grants-2013_08
特許番号
US08518943B2

関連ノート

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