4-[O-Benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine → 4-(3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamino)-3-methoxy-2-methylpyridine

HRID 1004

반응식

HRID 1004 반응식
C(O[N:9]([C:23]1[CH:28]=[CH:27][N:26]=[C:25]([CH3:29])[C:24]=1[O:30][CH3:31])[CH:10]1[CH2:22][CH2:21][C:13]2([O:18][CH2:17][C:16]([CH3:20])([CH3:19])[CH2:15][O:14]2)[CH2:12][CH2:11]1)C1C=CC=CC=1>CO.[Ni]>[CH3:19][C:16]1([CH3:20])[CH2:17][O:18][C:13]2([CH2:12][CH2:11][CH:10]([NH:9][C:23]3[CH:28]=[CH:27][N:26]=[C:25]([CH3:29])[C:24]=3[O:30][CH3:31])[CH2:22][CH2:21]2)[O:14][CH2:15]1

참가 물질

4

반응물 1

HCID 196939824-[O-Benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine

생성물 1

HCID 196939904-(3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamino)-3-methoxy-2-methylpyridine

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

6.5 g of 4-[O-benzyl-N-(3,3-dimethyl-1,5-dioxaspiro[5.5]undec-9-yl)hydroxylamino]-3-methoxy-2-methylpyridine in 70 ml of methanol are hydrogenated using 2 g of Raney nickel at normal pressure until absorption of hydrogen is complete. After filtering, the filtrate is concentrated and the product is dissolved in diisopropyl ether. Crystallization takes place on addition of hexane. 4.3 g=90%; m.p.: 45° C.

후처리

  1. customuntil absorption of hydrogen
  2. filtrationAfter filtering
  3. concentrationthe filtrate is concentrated
  4. dissolutionthe product is dissolved in diisopropyl ether
  5. customCrystallization
  6. additionon addition of hexane

출처 및 근거

ORD 기록
ord-f4dba46589654bd6a818f29b87cc4306
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723450

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