Diethyl Ether → 2-amino-4-(thien-2-yl)-4H-oxazol-5-one hydrochloride

HRID 64762노트

반응식

HRID 64762 반응식
S(Cl)([Cl:3])=O.[NH2:5][C:6]([NH:8][CH:9]([C:13]1[S:14][CH:15]=[CH:16][CH:17]=1)[C:10]([OH:12])=[O:11])=O.CCOCC>C(#N)C>[ClH:3].[NH2:5][C:6]1[O:11][C:10](=[O:12])[CH:9]([C:13]2[S:14][CH:15]=[CH:16][CH:17]=2)[N:8]=1

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 24386Thionyl ChlorideHCID 129116992-[(Aminocarbonyl)amino]-2-(thien-2-yl)acetic acid

생성물 1

HCID 198432152-amino-4-(thien-2-yl)-4H-oxazol-5-one hydrochloride수율 92%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Thionyl chloride (0.87 g, 7.3 mmol) was added to a suspension of 2-[(aminocarbonyl)amino]-2-(thien-2-yl) acetic acid (0.60 g, 3 mmol) in dry acetonitrile (17 ml) at 0°-5° C. under a nitrogen atmosphere. After 5 minutes dry ether (29 ml) was added and the resulting slurry was stirred for 10 minutes. The precipitate was then filtered under nitrogen, and washed well with ether. The product was dried in vacuo to afford 2-amino-4-(thien2-yl)-4H-oxazol-5-one hydrochloride (0.60 g, 92%) as a salmon pink powder; νmax (Nujol) 1878, 1745, 1725 cm-1.

후처리

  1. filtrationThe precipitate was then filtered under nitrogen
  2. washwashed well with ether
  3. customThe product was dried in vacuo

출처 및 근거

ORD 기록
ord-fa2d7e01c8574b83861ad9bf279007b1
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04609652

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