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Benzyltrimethylammonium hydroxide → (R)-4-Acetyl-1-((S)-1-(4-methoxyphenyl)ethyl)pyrrolidin-2-one

HRID 870553
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HRID 870553 반응식
[C:1]([CH:4]1[CH2:8][N:7]([C@H:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH3:18])=[CH:13][CH:12]=2)[CH3:10])[C:6](=[O:19])[CH2:5]1)(=[O:3])[CH3:2].[OH-].C([N+](C)(C)C)C1C=CC=CC=1>C(O)CCC>[C:1]([C@H:4]1[CH2:8][N:7]([C@H:9]([C:11]2[CH:12]=[CH:13][C:14]([O:17][CH3:18])=[CH:15][CH:16]=2)[CH3:10])[C:6](=[O:19])[CH2:5]1)(=[O:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 66854Benzyltrimethylammonium hydroxideHCID 580720164-Acetyl-1-[(1S)-1-(4-methoxyphenyl)ethyl]pyrrolidin-2-one

생성물 1

HCID 58071853(R)-4-Acetyl-1-((S)-1-(4-methoxyphenyl)ethyl)pyrrolidin-2-one

시약·촉매·용매 1

HCID 2631-Butanol용매

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온도
25 °C

실험 절차

103 g of a mixture of diastereoisomers (R/S)-4-acetyl-1-[(S)-1-(4-methoxyphenyl)-ethyl]-pyrrolidine-2-one is dissolved in 155 mL 1-butanol at 25° C. 18 mL benzyltrimethylammonium hydroxide (40% solution in methanol) is added. The solution is stirred for 30 minutes at 25° C. The solution is cooled to 0° C. Precipitation starts. The suspension is stirred for 15 minutes at 0° C. 100 mL n-heptane is added slowly and the suspension is stirred for 30 minutes at 0° C. The addition of 100 mL portions of n-heptane is repeated 4 times with subsequent stirring of the suspension at 0° C. for 30 minutes. The precipitate is isolated, washed with n-heptane and dried at 50° C.

후처리

  1. temperatureThe solution is cooled to 0° C
  2. customPrecipitation
  3. stirringThe suspension is stirred for 15 minutes at 0° C
  4. addition100 mL n-heptane is added slowly
  5. stirringthe suspension is stirred for 30 minutes at 0° C
  6. additionThe addition of 100 mL portions of n-heptane
  7. stirringwith subsequent stirring of the suspension at 0° C. for 30 minutes
  8. customThe precipitate is isolated
  9. washwashed with n-heptane
  10. customdried at 50° C.

출처 및 근거

ORD 기록
ord-6de35f45f6a640b585b5f5a165c13c45
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969568B2

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