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HCID 19024940, 화합물 → 4-Benzyl-2,2-bis(methoxymethyl)morpholine

HRID 1375050
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HRID 1375050 반응식
S(O)(O[CH2:5][CH2:6][NH:7][CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(=O)=O.[CH3:16][O:17][CH2:18][C:19]1([CH2:22][O:23][CH3:24])[CH2:21][O:20]1>O.[OH-].[Na+]>[CH2:8]([N:7]1[CH2:6][CH2:5][O:20][C:19]([CH2:18][O:17][CH3:16])([CH2:22][O:23][CH3:24])[CH2:21]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1
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참가 물질

5

반응물 2

HCID 19024940HCID 19024940, 화합물HCID 218250682-(Benzylamino)ethyl hydrogen sulfate

생성물 1

HCID 179638464-Benzyl-2,2-bis(methoxymethyl)morpholine수율 99%

시약·촉매·용매 2

HCID 962Water용매HCID 14798Sodium Hydroxide용매2회

실험 절차

To a solution of 2-(N-benzylamino)ethyl hydrogen sulfate (28 g) in a mixture of water (36.3 ml) and 40% sodium hydroxide aqueous solution (12.1 ml) was added 2,2-bis(methoxymethyl)oxirane (16.0 g) at room temperature over 30 minutes. After stirring at room temperature for 87 hours, 40% sodium hydroxide aqueous solution (73 ml) was added dropwise to the mixture over 20 minutes. The mixture was stirred at room temperature for 1 hour and at 40° C. for 20 hours, and extracted with ethyl acetate (100 ml×3). The organic layer was extracted with 1N hydrochloric acid (×6). The combined extracts were neutralized with sodium hydroxide, and then added sodium chloride, and extracted with ethyl acetate (100 ml×3). The combined extracts were washed with brine, dried over magnesium sulfate, and evaporated under reduced pressure to give 4-benzyl-2,2-dimethoxymethylmorpholine (31.79 g) as an orange oil.

후처리

  1. stirringThe mixture was stirred at room temperature for 1 hour and at 40° C. for 20 hours
  2. extractionextracted with ethyl acetate (100 ml×3)
  3. extractionThe organic layer was extracted with 1N hydrochloric acid (×6)
  4. extractionadded sodium chloride, and extracted with ethyl acetate (100 ml×3)
  5. washThe combined extracts were washed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b7dbdc7b68c84f6ab23b1c65a712c949
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07166598B2

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