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

HRID 1896387

반응식

HRID 1896387 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb9515b5a4394681a0b7360f5cfcf5e3
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518943B2

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