HCID 13136924、化合物 → HCID 13136926、化合物

HRID 851198ノート

反応式

HRID 851198 の反応式
[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

参加物

6

反応物 2

HCID 13136924HCID 13136924、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 13136926HCID 13136926、化合物収率 81.2%

試薬・触媒・溶媒 3

HCID 935Nickel触媒2 回HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-48376c66ea3949c982275571ed8d9c8c
出典データセット
uspto-grants-1983_05
特許番号
US04382939

反応ノート

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