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Sodium Carbonate → 5-(cyclopropylmethyl)-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazole-4-carboxylic acid

HRID 1717291
ノート
印刷プレビュー

反応式

HRID 1717291 の反応式
[CH:1]1([CH2:4][C:5](=O)[CH2:6][C:7]([O:9]CC)=[O:8])[CH2:3][CH2:2]1.[N:13]([C:16]1[CH:26]=[CH:25][C:19]([C:20]([NH:22][CH2:23][CH3:24])=[O:21])=[CH:18][CH:17]=1)=[N+:14]=[N-:15].[O-]CC.[Na+].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[CH:1]1([CH2:4][C:5]2[N:13]([C:16]3[CH:17]=[CH:18][C:19]([C:20]([NH:22][CH2:23][CH3:24])=[O:21])=[CH:25][CH:26]=3)[N:14]=[N:15][C:6]=2[C:7]([OH:9])=[O:8])[CH2:2][CH2:3]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 2723922Sodium ethoxideHCID 21099281Ethyl 4-cyclopropyl-3-oxobutanoateHCID 594322264-azido-N-ethylbenzamide

生成物 1

HCID 685122045-(cyclopropylmethyl)-1-{4-[(ethylamino)carbonyl]phenyl}-1H-1,2,3-triazole-4-carboxylic acid収率 101.7%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒
2 回

反応条件

温度
80 °C

実験手順

Ethyl 4-cyclopropyl-3-oxobutyrate (1.20 g, 7.05 mmol, 1.2 eq.) obtained in Example 96a) and 4-azido-N-ethylbenzamide (1.20 g, 5.88 mmol) were dissolved in ethanol (25 ml), sodium ethoxide (556 mg, 7.35 mmol, 1.25 eq.) was added, and the mixture was stirred at room temperature for 30 min and at 80° C. for 2.5 hr. 2% Aqueous sodium carbonate solution (40 ml) was added to the reaction mixture, ethanol was evaporated, and the residue was diluted with water (20 ml) and washed twice with ethyl acetate-hexane (2:1, 50 ml). The organic layer was extracted with 1% aqueous sodium carbonate solution (20 ml). The aqueous layers were combined, acidified (pH<3) with 6N hydrochloric acid, and stood still at 5° C. The precipitate was collected by filtration, washed with cold water and dried to give the title compound as a pale-brown powder (1.88 g, 5.98 mmol, 101.7%).

後処理

  1. customwas evaporated
  2. additionthe residue was diluted with water (20 ml)
  3. washwashed twice with ethyl acetate-hexane (2:1, 50 ml)
  4. extractionThe organic layer was extracted with 1% aqueous sodium carbonate solution (20 ml)
  5. customstood still at 5° C
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with cold water
  8. customdried

出典と根拠

ORDレコード
ord-48dcebec2fa6453fa2e17c2eff64d7a1
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803822B2

反応ノート

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