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Hydrochloric Acid → (S)-N,N-Dimethyl(pyrrolidin-2-yl)methanamine hydrochloride

HRID 1366669
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HRID 1366669 반응식
[CH3:1][N:2]([CH3:16])[CH2:3][C@@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1CC1C=CC=CC=1.[ClH:17]>CO>[ClH:17].[CH3:1][N:2]([CH3:16])[CH2:3][C@@H:4]1[CH2:8][CH2:7][CH2:6][NH:5]1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 66936141N,N-dimethyl-1-[(2S)-1-(phenylmethyl)-2-pyrrolidinyl]methanamine

생성물 1

HCID 53346548(S)-N,N-Dimethyl(pyrrolidin-2-yl)methanamine hydrochloride수율 119.8%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

N,N-Dimethyl-1-[(2S)-1-(phenylmethyl)-2-pyrrolidinyl]methanamine (3.730 g, 17.08 mmol) was dissolved in a mixture of MeOH (100 mL) and 1N HCl (35 mL, 34.16 mmol), degassed and placed under argon. 10% Pd/C (1.119 g) was added, and the contents were thoroughly degassed and placed under a hydrogen balloon for 2 h. The contents were then degassed, and the Pd/C was removed by filtration through a fiberglass filter, washing with MeOH. The filtrate was concentrated in vacuo to provide pure N,N-dimethyl-1-[(2S)-2-pyrrolidinyl]methanamine hydrochloride (3.3701 g, >99%). LCMS: (M+H)+: 129.1.

후처리

  1. customdegassed
  2. addition10% Pd/C (1.119 g) was added
  3. customthe contents were thoroughly degassed
  4. customfor 2 h
  5. customThe contents were then degassed
  6. customthe Pd/C was removed by filtration through a fiberglass
  7. filtrationfilter
  8. washwashing with MeOH
  9. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-440e6e5a58ad45cdabb196372a586223
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893056B2

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