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

HRID 1666708

反応式

HRID 1666708 の反応式
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

参加物

4

反応物 3

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

生成物 1

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

反応条件

温度
40 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e6151e03b1cc4ccc8e0cef04df781c73
出典データセット
uspto-grants-2011_10
特許番号
US08044078B2

関連ノート

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