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Triethylamine → Methyl 2-methyl-4,5-dihydro-1,3-oxazole-4-carboxylate

HRID 880517
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인쇄 미리보기

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HRID 880517 반응식
[CH2:1](N(CC)CC)[CH3:2].CCl.[NH2:10][C@H:11]([C:14]([OH:16])=[O:15])[CH2:12][OH:13].Cl.[CH2:18](OC(=N)C)C>ClCCl>[CH3:1][C:2]1[O:13][CH2:12][CH:11]([C:14]([O:16][CH3:18])=[O:15])[N:10]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 86654677HCID 86654677, 화합물

생성물 1

HCID 10844497Methyl 2-methyl-4,5-dihydro-1,3-oxazole-4-carboxylate수율 72.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Triethylamine (5.86 g, 58.01 mmol) was added to a suspension of L-serine methyl hydrochloride (4.5 g, 29.03 mmol) and ethylacetimidate hydrochloride (4.3 g, 34.95 mmol) in dichloromethane (40 mL) at 0° C. over a period of 20 min. The mixture was then stirred at ambient temperature for 18 h. The suspension was filtered and washed with diethyl ether. The solid which precipitated from the filtrate was again filtered and washed with diethyl ether. The resulting filtrate was dried over anhydrous sodium sulfate and concentrated in vacuo to afford methyl 2-methyl-4,5-dihydrooxazole-4-carboxylate (3 g, 72%) as a liquid.

후처리

  1. filtrationThe suspension was filtered
  2. washwashed with diethyl ether
  3. customThe solid which precipitated from the filtrate
  4. filtrationwas again filtered
  5. washwashed with diethyl ether
  6. dry with materialThe resulting filtrate was dried over anhydrous sodium sulfate
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-5ba83008ff2e46b78f47f806272b42eb
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08993574B2

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