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

HRID 635784

반응식

HRID 635784 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

5-Chloro-2-methyl-6-nitrobenzoxazole (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 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 6-amino-5-chloro-2-methylbenzoxazole (1), 22 g.

후처리

  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

출처 및 근거

ORD 기록
ord-8bfb09c16556432eaf7c606f1664e43d
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06190850B1

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