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Chloroacetyl chloride → Isopropyl 2-(morpholinoamino)-4-oxo-4,5-dihydrofuran-3-carboxylate

HRID 402736
ノート
印刷プレビュー

反応式

HRID 402736 の反応式
C(O[C:5]1[O:6][CH2:7][C:8](=[O:16])[C:9]=1[C:10]([O:12][CH:13]([CH3:15])[CH3:14])=[O:11])(C)C.C(OC(C)C)(=O)CC(OC(C)C)=O.ClCC(Cl)=O.[NH2:35][N:36]1[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1>C(O)C>[O:39]1[CH2:40][CH2:41][N:36]([NH:35][C:5]2[O:6][CH2:7][C:8](=[O:16])[C:9]=2[C:10]([O:12][CH:13]([CH3:14])[CH3:15])=[O:11])[CH2:37][CH2:38]1
参加物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 6577Chloroacetyl chlorideHCID 20315N-AminomorpholineHCID 83223Diisopropyl malonateHCID 51050080Isopropyl 2-isopropoxy-4-oxo-4,5-dihydrofuran-3-carboxylate

生成物 1

HCID 86708411Isopropyl 2-(morpholinoamino)-4-oxo-4,5-dihydrofuran-3-carboxylate

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

To a solution of isopropyl 2-isopropoxy-4-oxo-4,5-dihydrofuran-3-carboxylate (12.2 g, 53.6 mmol), which similarly prepared according to the procedure described in the Example 74, Third step using diisopropyl malonate and chloroacetyl chloride, in ethanol (45 mL), 4-aminomorpholine (5.7 mL, 59.2 mmol) was added at ambient temperature. The mixture was stirred for 18 h. The solvent was removed under reduced pressure, and the crude product was suspended in methyl tert-butyl ether, then the precipitate was collected by filtration, washed with methyl tert-butyl ether and hexane then dried to afford isopropyl 2-(morpholinoamino)-4-oxo-4,5-dihydrofuran-3-carboxylate as solid (11.2 g, y. 75%).

後処理

  1. customThe solvent was removed under reduced pressure
  2. filtrationthe precipitate was collected by filtration
  3. washwashed with methyl tert-butyl ether and hexane
  4. customthen dried

出典と根拠

ORDレコード
ord-9401091bbd5f4cd7bb2ee7a7c88ee7d2
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08742113B2

反応ノート

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