2,2,2-Trichloroethyl chloroformate → 2,2,2-Trichloroethyl benzo[d]isoxazol-3-ylcarbamate

HRID 1098605

反応式

HRID 1098605 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([NH2:10])=[N:2]1.[C:11](Cl)([O:13][CH2:14][C:15]([Cl:18])([Cl:17])[Cl:16])=[O:12]>>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[C:3]([NH:10][C:11](=[O:12])[O:13][CH2:14][C:15]([Cl:18])([Cl:17])[Cl:16])=[N:2]1

参加物

3

反応物 2

HCID 870632,2,2-Trichloroethyl chloroformateHCID 27797491,2-Benzoxazol-3-amine

生成物 1

HCID 667289402,2,2-Trichloroethyl benzo[d]isoxazol-3-ylcarbamate

実験手順

Using General Method A, benzo[d]isoxazol-3-amine (500 mg, 3.37 mmol) and Troc-Cl (1.185 g, 5.59 mmol) were combined, purified by column chromatography (ethyl acetate/hexanes), triturated with hexanes (30 mL), filtered and dried to afford 2,2,2-trichloroethyl benzo[d]isoxazol-3-ylcarbamate. 1H NMR (300 MHz, DMSO-d6): δ 5.15 (s, 2 H), 7.50 (t, 1 H), 7.77-7.83 (m, 2 H), 8.16 (d, 1 H), 11.51 (s, 1 H); MS (ESI) m/z: 310.9 (M+H+).

後処理

  1. custompurified by column chromatography (ethyl acetate/hexanes)
  2. customtriturated with hexanes (30 mL)
  3. filtrationfiltered
  4. customdried

出典と根拠

ORDレコード
ord-7db931415d854f5faa498a770089f0c0
出典データセット
uspto-grants-2012_03
特許番号
US08143293B2

関連ノート

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