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Pyridine → HCID 73867328、化合物

HRID 1111043
ノート
印刷プレビュー

反応式

HRID 1111043 の反応式
[CH2:1]([O:3][C:4](=[O:11])[CH2:5][NH:6][CH2:7][CH:8]=[CH:9][CH3:10])[CH3:2].N([CH2:15][CH2:16][CH2:17][C:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=O)=C=O.Cl.[NH2:27][OH:28].C([O:34][CH3:35])(OC)OC.[N:36]1C=CC=CC=1>C1COCC1>[OH:28][N:27]=[C:18]([C:20]1[CH:21]=[CH:22][C:23]([NH:36][C:35]([N:6]([CH2:7][CH:8]=[CH:9][CH3:10])[CH2:5][C:4]([O:3][CH2:1][CH3:2])=[O:11])=[O:34])=[CH:24][CH:25]=1)[CH2:17][CH2:16][CH3:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 1049PyridineHCID 9005Trimethyl orthoformateHCID 443297Hydroxyamine hydrochlorideHCID 22154871HCID 22154871、化合物HCID 53851665HCID 53851665、化合物

生成物 1

HCID 73867328HCID 73867328、化合物

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A solution of 0.02 mol N-2-butenylglycine ethyl ester, prepared as described by S. B. Hyeon, I. Nagai, H. Iesaka, T. Kajita, and M. Furushima in European Patent Application No. 181,494, in 40 mL of THF is added dropwise to a solution of 0.02 mol of 4-isocyanatobutyrophenone, prepared as described by E. E. Kilbourn, D. L. Peardon, and J. E. Ware in U.S. Pat. No. 3,931,203, and 5 mL of pyridine in 40 mL of THF, and the reaction mixture is stirred for 3 hours. The solvent is then removed by rotary evaporator. The residue is dispersed in 50 mL of CH3OH, and 0.022 mol of hydroxylamine hydrochloride and 0.06 mol of trimethyl orthoformate are added. The reaction mixture is heated to reflux for 1 hour. The solvent is removed by rotary evaporator to give the product, N-[4-(1-hydroxyiminobutyl)phenyl]-N'-(2-butenyl)-N'-ethoxycarbonylmethylurea.

後処理

  1. customprepared
  2. customThe solvent is then removed by rotary evaporator
  3. additionThe residue is dispersed in 50 mL of CH3OH
  4. temperatureThe reaction mixture is heated
  5. temperatureto reflux for 1 hour
  6. customThe solvent is removed by rotary evaporator

出典と根拠

ORDレコード
ord-513c85448db748bcbd000c144049db03
出典データセット
uspto-grants-1990_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04977272

反応ノート

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