HCID 5156493、化合物 → HCID 10559687、化合物

HRID 968491ノート

反応式

HRID 968491 の反応式
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:9]2[CH2:8][CH2:7][CH2:6][CH2:5][C:4]=2[N:3]=1.[NH3:15].CO>>[N+:12]([C:11]1[C:2]([NH2:15])=[N:3][C:4]2[CH2:5][CH2:6][CH2:7][CH2:8][C:9]=2[CH:10]=1)([O-:14])=[O:13]

参加物

3

反応物 2

HCID 5156493HCID 5156493、化合物HCID 21705897Ammonia methanol

生成物 1

HCID 10559687HCID 10559687、化合物

反応条件

温度
120 °C

実験手順

A mixture of intermediate (9) (0.0658 mol) in NH3/CH3OH 7N (60 ml) was stirred at 120° C. for 12 hours in an autoclave. The solvent was evaporated till dryness. The residue was taken up in 2-propanone. The precipitate was filtered off and dried, yielding 8.6 g 5,6,7,8-tetrahydro-3-nitro-2-quinolinamine (intermediate 10). d) A mixture of intermediate (10) (0.031 mol) in methanol (100 ml) was hydrogenated at room temperature under a 3.105 Pa (3 bar) pressure for 30 minutes in a Parr apparatus. After uptake of hydrogen (3 equivalents), the catalyst was filtered through celite, rinced with methanol and the filtrate was evaporated till dryness. The product was used with further purification, yielding 5.07 g 5,6,7,8-tetrahydro-2,3-quinolinediamine (intermediate 11).

後処理

  1. customThe solvent was evaporated till dryness
  2. filtrationThe precipitate was filtered off
  3. customdried

出典と根拠

ORDレコード
ord-3eacdbdeca0a4819ad0f2cb810565eeb
出典データセット
uspto-grants-2007_12
特許番号
US07304052B2

反応ノート

読み込み中…