Water → HCID 86680394、化合物

HRID 83585ノート

反応式

HRID 83585 の反応式
[CH3:1][O:2][C:3]1[CH:20]=[C:19]([O:21][CH3:22])[CH:18]=[CH:17][C:4]=1[CH2:5][N:6]1[CH2:12][CH:11]([C:13]([OH:15])=O)[C:8]2([CH2:10][CH2:9]2)[C:7]1=[O:16].[CH2:23]([C@@H:30]1[CH2:34][O:33][C:32](=[O:35])[NH:31]1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.CCN=C=NCCCN(C)C.Cl.O>C(Cl)(Cl)Cl.CN(C1C=CN=CC=1)C>[CH2:23]([C@@H:30]1[CH2:34][O:33][C:32](=[O:35])[N:31]1[C:13]([CH:11]1[C:8]2([CH2:9][CH2:10]2)[C:7](=[O:16])[N:6]([CH2:5][C:4]2[CH:17]=[CH:18][C:19]([O:21][CH3:22])=[CH:20][C:3]=2[O:2][CH3:1])[CH2:12]1)=[O:15])[C:24]1[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

7

反応物 4

HCID 962WaterHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 2734969(R)-4-Benzyl-2-oxazolidinoneHCID 866803935-(2,4-Dimethoxybenzyl)-4-oxo-5-azaspiro[2.4]heptane-7-carboxylic Acid

生成物 1

HCID 86680394HCID 86680394、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6212Chloroform溶媒

実験手順

To a solution of 5-(2,4-dimethoxybenzyl)-4-oxo-5-azaspiro[2.4]heptane-7-carboxylic acid (1.59 g) in chloroform (16 ml) were sequentially added (R)-4-benzyl-2-oxazolidinone (1.11 g), WSC.HCl (1.20 g) and N,N-dimethyl-4-aminopyridine (318 mg) at room temperature, and the mixture was stirred for 4 hours. To this reaction mixture was added water, and the organic layer was separated from the solution, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1) to separate a low-polarity component as the titled compound (1.39 g).

後処理

  1. customat room temperature
  2. customthe organic layer was separated from the solution
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=2/1)
  5. customto separate a low-polarity component as the titled compound (1.39 g)

出典と根拠

ORDレコード
ord-f9a91d34ee9e4421b589697e0c2533fa
出典データセット
uspto-grants-2014_09
特許番号
US08846746B2

反応ノート

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