HCID 13136924, 화합물 → HCID 13136926, 화합물

HRID 851198노트

반응식

HRID 851198 반응식
[CH3:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]2[C:11]3[CH2:16][CH2:15][NH:14][CH2:13][C:12]=3[C:17](=[O:19])[O:18][C:4]=2[CH:3]=1.[H][H]>CN(C)C=O.CO.[Ni]>[NH2:8][C:7]1[C:2]([CH3:1])=[CH:3][C:4]2[O:18][C:17](=[O:19])[C:12]3[CH2:13][NH:14][CH2:15][CH2:16][C:11]=3[C:5]=2[CH:6]=1

참가 물질

6

반응물 2

HCID 13136924HCID 13136924, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 13136926HCID 13136926, 화합물수율 81.2%

시약·촉매·용매 3

HCID 935Nickel촉매2회HCID 887Methanol용매HCID 6228Dimethylformamide용매2회

실험 절차

A solution of 1,2,3,4-tetrahydro-8-methyl-9-nitro-5H-[1]benzopyrano[3,4-c]pyridin-5-one (6.0 g, 0.023 moles) in N,N-dimethylformamide (100 ml) and methanol (50 ml) is hydrogenated at 50 psi in the presence of Raney Nickel (0.5 g) at room temperature for 20 hours. Additional Raney Nickel (0.5 g) in N,N-dimethylformamide (50 ml) is then added, and hydrogenation resumed until hydrogen uptake ceases. The catalyst is filtered off and rinsed with warm N,N-dimethylformamide. The filtrate is concentrated under reduced pressure and filtered to afford the product (4.3 g), mp 283°-284° C.

후처리

  1. filtrationThe catalyst is filtered off
  2. washrinsed with warm N,N-dimethylformamide
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. filtrationfiltered

출처 및 근거

ORD 기록
ord-48376c66ea3949c982275571ed8d9c8c
출처 데이터셋
uspto-grants-1983_05
특허 번호
US04382939

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