Chloroform → Methyl-3-[(1,3-benzoxazol-2-yl)amino]-2-methylpropionate

HRID 1666708

반응식

HRID 1666708 반응식
Cl.[NH2:2][CH2:3][CH:4]([CH3:9])[C:5]([O:7][CH3:8])=[O:6].C(Cl)(Cl)Cl.Cl[C:15]1[O:16][C:17]2[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=2[N:19]=1>>[CH3:8][O:7][C:5](=[O:6])[CH:4]([CH3:9])[CH2:3][NH:2][C:15]1[O:16][C:17]2[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=2[N:19]=1

참가 물질

4

반응물 3

HCID 6212ChloroformHCID 119862-ChlorobenzoxazoleHCID 13063725Methyl 3-amino-2-methylpropanoate hydrochloride

생성물 1

HCID 67445136Methyl-3-[(1,3-benzoxazol-2-yl)amino]-2-methylpropionate수율 70.4%

반응 조건

온도
40 °C

실험 절차

To the suspension of 0.55 g (4 mmol) methy 3-amino-2-methylpropionate hydrogen chloride salt and 4 ml chloroform 0.52 g (5.2 mmol) triethylamine and 0.3 g (2 mmol) 2-chloro-1,3-benzoxazole are added and the mixture is stirred at 40° C. for 4 hours and at room temperature for 12 hours. The chloroform solution is washed with water, citric acid solution and water, dried over sodium sulfate and evaporated in vacuum. The residue is treated with hexane, the crystals are filtered off and washed. 0.33 g title compound is obtained as white crystals. Mp: 89-90° C.

후처리

  1. additionare added
  2. washThe chloroform solution is washed with water, citric acid solution and water
  3. dry with materialdried over sodium sulfate
  4. customevaporated in vacuum
  5. additionThe residue is treated with hexane
  6. filtrationthe crystals are filtered off
  7. washwashed

출처 및 근거

ORD 기록
ord-e6151e03b1cc4ccc8e0cef04df781c73
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044078B2

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