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Sodium Hydroxide → 9-Amino-N11-ethyl-N6-methyl-6,11-dihydro-5H-pyrido(2,3-b)(1,5)benzodiazepin-5-one

HRID 1898881
ノート
印刷プレビュー

反応式

HRID 1898881 の反応式
[CH2:1]([N:3]1[C:9]2[CH:10]=[C:11]([N+:14]([O-])=O)[CH:12]=[CH:13][C:8]=2[N:7]([CH3:17])[C:6](=[O:18])[C:5]2[CH:19]=[CH:20][CH:21]=[N:22][C:4]1=2)[CH3:2].O.O.Cl[Sn]Cl.C(=O)(O)[O-].[Na+].[OH-].[Na+]>C(O)(=O)C.Cl>[NH2:14][C:11]1[CH:12]=[CH:13][C:8]2[N:7]([CH3:17])[C:6](=[O:18])[C:5]3[CH:19]=[CH:20][CH:21]=[N:22][C:4]=3[N:3]([CH2:1][CH3:2])[C:9]=2[CH:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 44701211-Ethyl-6-methyl-9-nitropyrido(3,2-C)(1,5)benzodiazepin-5-oneHCID 516892Sodium Bicarbonate

生成物 1

HCID 4532829-Amino-N11-ethyl-N6-methyl-6,11-dihydro-5H-pyrido(2,3-b)(1,5)benzodiazepin-5-one収率 44.7%

試薬・触媒・溶媒 2

HCID 176
Acetic Acid
溶媒
HCID 313Hydrochloric Acid溶媒

実験手順

To a solution of 0.3 g (1 mmol) of 6,11-dihydro-11-ethyl-6-methyl-9-nitro-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one in acetic acid (5 ml) was added a solution of SnCl2.2H2O (1.7 g) in concentrated hydrochloric acid (2.2 ml). The mixture was stirred at room temperature for 6 hours, and then poured into a saturated sodium bicarbonate solution and made basic with aqueous sodium hydroxide. The aqueous phase was then extracted with ethyl acetate, dried (MgSO4), filtered and concentrated in vacuo. The solid material obtained was recrystallized from ethyl acetate to give 0.12 g (44% of theory) of 6,11-dihydro-9-amino-11-ethyl-6-methyl-5H-pyrido[2,3-b][1,5]benzodiazepin-5-one, m.p. 193°-195° C.

後処理

  1. extractionThe aqueous phase was then extracted with ethyl acetate
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe solid material obtained
  6. customwas recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-fe2c4575845149408e5dd51e3bbd73e2
出典データセット
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05571809

反応ノート

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