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Hydrochloric Acid → Morpholine, 2,2-bis(methoxymethyl)-, hydrochloride (1:1)

HRID 1910401
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HRID 1910401 반응식
C([N:8]1[CH2:13][CH2:12][O:11][C:10]([CH2:17][O:18][CH3:19])([CH2:14][O:15][CH3:16])[CH2:9]1)C1C=CC=CC=1.[ClH:20]>CO.[OH-].[OH-].[Pd+2]>[ClH:20].[CH3:16][O:15][CH2:14][C:10]1([CH2:17][O:18][CH3:19])[O:11][CH2:12][CH2:13][NH:8][CH2:9]1
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 179638464-Benzyl-2,2-bis(methoxymethyl)morpholine

생성물 1

HCID 17964181Morpholine, 2,2-bis(methoxymethyl)-, hydrochloride (1:1)

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매

실험 절차

To a solution of 4-benzyl-2,2-bis(methoxymethyl)morpholine (6 g) and conc HCl (2.41 ml) in MeOH (60 ml) was added 20% palladium hydroxide on charcoal (1.2 g), and the whole was stirred for 2 hours at room temperature under hydrogen (2.0 atm). The catalyst was filtered off, and the filtrate was concentrated under reduced pressure to give 2,2-bis(methoxymethyl)morpholine hydrochloride (3.6 g). The obtained HCl salt was diluted with CH2Cl2 and washed with 1N—NaOH. The organic phase was concentrated under reduced pressure to give gave free form, which was used for next reaction.

후처리

  1. filtrationThe catalyst was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-dca5a68aff94456cbc74e9d475a44c68
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08603975B2

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