Ethanol → Ethyl 2-(1-benzylpyrrolidin-2-yl)acetate

HRID 1253499노트

반응식

HRID 1253499 반응식
[CH2:1]([OH:3])[CH3:2].S(=O)(=O)(O)O.[CH2:9]([N:16]1[CH2:20][CH2:19][CH2:18][CH:17]1[CH2:21][C:22]#N)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(=O)([O-])[O-:25].[Na+].[Na+]>O>[CH2:9]([N:16]1[CH2:20][CH2:19][CH2:18][CH:17]1[CH2:21][C:22]([O:3][CH2:1][CH3:2])=[O:25])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 226628942-(1-Benzylpyrrolidin-2-yl)acetonitrile

생성물 1

HCID 11010289Ethyl 2-(1-benzylpyrrolidin-2-yl)acetate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Into a 3,000 ml roundbottom flask, was placed ethanol (479. g, 10.4 mol), followed by concentrated sulfuric acid (417 g, 4.17 mol). To the mixture was added 2-(1-benzylpyrrolidin-2-yl)acetonitrile (139. g, 695. mmol). The resulting solution was heated to reflux for 4 hours. After cooling to ambient temperature, the solution was diluted with 3,000 ml of water. Adjustment of the pH to 9 was accomplished by the addition of solid sodium carbonate. The resulting solution was extracted three times with 2,000 ml of ethyl acetate and the combined organic layers were concentrated to afford ethyl 2-(1-benzylpyrrolidin-2-yl)acetate, which was used without additional purification.

후처리

  1. customInto a 3,000 ml roundbottom flask, was placed
  2. temperatureThe resulting solution was heated
  3. temperatureto reflux for 4 hours
  4. extractionThe resulting solution was extracted three times with 2,000 ml of ethyl acetate
  5. concentrationthe combined organic layers were concentrated

출처 및 근거

ORD 기록
ord-4db88a77b83d4baf8db3eb6e42c8cd30
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08455477B2

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