Potassium Carbonate → HCID 68874499、化合物

HRID 2366630ノート

反応式

HRID 2366630 の反応式
[N+:1]([C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[NH:14][CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=[CH:9][CH:8]=2)([O-])=O.S(S([O-])=O)([O-])=O.[Na+].[Na+].C(=O)([O-])[O-].[K+].[K+]>CC[N+]1C=CC(C2C=C[N+](CC)=CC=2)=CC=1.[Br-].[Br-]>[NH2:1][C:4]1[CH:5]=[N:6][C:7]2[C:12]([C:13]=1[NH:14][CH2:15][CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:11][CH:10]=[CH:9][CH:8]=2

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 24489Sodium Dithionite2 回HCID 68873567HCID 68873567、化合物

生成物 1

HCID 68874499HCID 68874499、化合物

試薬・触媒・溶媒 1

HCID 114742621,1'-Diethyl-4,4'-bipyridinium dibromide触媒

実験手順

Ethyl N-(3-nitroquinolin-4-yl)-β-alaninate (41.6 g, 144 mmol, prepared as described in Part A of Example 15) was treated with sodium hydrosulfite (87.62 g, 503.3 mmol), potassium carbonate (78.5 g, 568 mmol), and ethyl viologen dibromide (0.54 g, 1.4 mmol) according to a modification of the method described in Part A of Example 8. After the reaction was stirred overnight, additional sodium hydrosulfite (5.0 g, 29 mmol) was added, and the reaction was stirred for one additional hour. The organic layer was separated, washed with water (5×200 mL), dried over magnesium sulfate, filtered, and concentrated under reduced pressure to provide 33.3 g of ethyl N-(3-aminoquinolin-4-yl)-β-alaninate.

後処理

  1. stirringthe reaction was stirred for one additional hour
  2. customThe organic layer was separated
  3. washwashed with water (5×200 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-0821a5dc4e1448b6b1a9bf8301707a46
出典データセット
uspto-grants-2014_04
特許番号
US08697873B2

反応ノート

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