Hydrochloric Acid → HCID 19973181、化合物

HRID 1080470ノート

反応式

HRID 1080470 の反応式
CC([N:5]([CH2:9][C:10]([NH:12][N:13]1[CH:17]=[CH:16][CH:15]=[C:14]1[C:18](=[O:20])[CH3:19])=[O:11])C(=O)[O-])(C)C.[ClH:21].CCOC(C)=O.CCCCCC>C(OCC)(=O)C.C(O)(C)C>[ClH:21].[C:18]([C:14]1[N:13]([NH:12][C:10](=[O:11])[CH2:9][NH2:5])[CH:17]=[CH:16][CH:15]=1)(=[O:20])[CH3:19]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 21226206Ethyl acetate hexaneHCID 867474421,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate

生成物 1

HCID 19973181HCID 19973181、化合物

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a stirred solution consisting of 1,1-dimethylethyl-[2-[(2-acetyl-1H-pyrrol-1-yl)amino]-2-oxoethyl]carbamate (5.90 g) in ethyl acetate (45 ml) and isopropanol (35 ml) was added ethereal HCl (1.7M, excess). The resulting suspension was gently heated until the reaction mixture was homogeneous. After stirring for 24 hours at room temperature, the reaction appeared complete by TLC (silica gel, 50% EtOAc/hexane). The solid product was collected by filtration under nitrogen and recrystallized from methanol/ether to afford 3.30 g of the product, m.p. 179°-182° C.

後処理

  1. temperatureThe resulting suspension was gently heated until the reaction mixture
  2. filtrationThe solid product was collected by filtration under nitrogen
  3. customrecrystallized from methanol/ether

出典と根拠

ORDレコード
ord-ee85940649184cf9bc65171e7bc9dc51
出典データセット
uspto-grants-1996_12
特許番号
US05580987

反応ノート

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