1-Octanol → HCID 54534880、化合物

HRID 1073299ノート

反応式

HRID 1073299 の反応式
[C:1]([N:11]1[CH2:16][CH2:15][CH:14]([C:17]([OH:19])=[O:18])[CH2:13][CH2:12]1)([O:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:2].C1(N=C=NC2CCCCC2)CCCCC1.[CH2:35](O)[CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42]>C(Cl)Cl.N1(C2C=CN=CC=2)CCCC1>[C:1]([N:11]1[CH2:16][CH2:15][CH:14]([C:17]([O:19][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH3:42])=[O:18])[CH2:13][CH2:12]1)([O:3][CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:2]

参加物

6

反応物 3

HCID 9571-OctanolHCID 10868DicyclohexylcarbodiimideHCID 7364891-Carbobenzoxy-4-piperidinecarboxylic Acid

生成物 1

HCID 54534880HCID 54534880、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 755674-Pyrrolidinopyridine溶媒

反応条件

温度
2.5 °C

実験手順

13.2 parts by weight of 1-carbobenzoxypiperidine-4-carboxylic acid are dissolved in 150 parts by volume of methylene chloride, 8 parts by volume of n-octanol and 0.7 part by weight of 4-pyrrolidinopyridine are added, and the mixture is cooled to 0 to 5° C. 12.0 parts by weight of dicyclohexylcarbodiimide are added, and the mixture is stirred at 5° C. for 2 hours and at room temperature for 4 hours. The mixture is left to stand overnight, the precipitated dicyclohexylurea is filtered off with suction (11.3 parts by weight), the solvent is stripped off in vacuo, the residue is stirred with diisopropyl ether in order to remove residual dicyclohexylurea and filtered, and the solvent is stripped off. 21 parts by weight of an oily residue are obtained. The residue is chromatographed on 1070 parts by weight of silica gel using CH2Cl2 /5% of methanol. 9.8 parts by weight of the compound (A) are obtained as an oil. ##STR42## 4-decyloxyphenoxy(4-benzoyl) chloroformate =(B)

後処理

  1. additionare added
  2. waitThe mixture is left
  3. waitto stand overnight
  4. filtrationthe precipitated dicyclohexylurea is filtered off with suction (11.3 parts by weight)
  5. stirringthe residue is stirred with diisopropyl ether in order
  6. customto remove residual dicyclohexylurea
  7. filtrationfiltered
  8. custom21 parts by weight of an oily residue are obtained
  9. customThe residue is chromatographed on 1070 parts by weight of silica gel

出典と根拠

ORDレコード
ord-f791ce0f76aa475ba378c32a0c180bd0
出典データセット
uspto-grants-1990_11
特許番号
US04968798

反応ノート

読み込み中…