5-Chloro-2-methyl-6-nitro-1,3-benzoxazole → 2-Methyl-5-chloro-6-benzoxazolamine

HRID 411954

反応式

HRID 411954 の反応式
[Cl:1][C:2]1[C:3]([N+:12]([O-])=O)=[CH:4][C:5]2[O:9][C:8]([CH3:10])=[N:7][C:6]=2[CH:11]=1>O1CCCC1>[NH2:12][C:3]1[C:2]([Cl:1])=[CH:11][C:6]2[N:7]=[C:8]([CH3:10])[O:9][C:5]=2[CH:4]=1

参加物

3

反応物 1

HCID 27644555-Chloro-2-methyl-6-nitro-1,3-benzoxazole

生成物 1

HCID 112754042-Methyl-5-chloro-6-benzoxazolamine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Compound (2), (30 g), was dissolved in tetrahydrofuran (150 mL), and Raney-Nickel which had been pre-washed with water (×3) and tetrahydrofuran (×3), was added. The mixture was then hydrogenated at room temperature and 352 kg/dm2 (50 psi) of hydrogen. The reaction is complete in approximately 1.5 hours. After this period, the catalyst is filtered off and the solution concentrated under reduced pressure. The residue is triturated with heptane, cooled and the solid filtered off. Yield 22 g.

後処理

  1. washRaney-Nickel which had been pre-washed with water (×3) and tetrahydrofuran (×3)
  2. additionwas added
  3. customwas then hydrogenated at room temperature
  4. waitAfter this period
  5. filtrationthe catalyst is filtered off
  6. concentrationthe solution concentrated under reduced pressure
  7. customThe residue is triturated with heptane
  8. temperaturecooled
  9. filtrationthe solid filtered off

出典と根拠

ORDレコード
ord-498e10bbd86a4e8c90610cd9b296b4ea
出典データセット
uspto-grants-2003_05
特許番号
US06562558B1

関連ノート

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