1-Octanol → HCID 54534880, 화합물

HRID 1073299노트

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HRID 1073299 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 54534880HCID 54534880, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 755674-Pyrrolidinopyridine용매

반응 조건

온도
2.5 °C

실험 절차

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)

후처리

  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

출처 및 근거

ORD 기록
ord-f791ce0f76aa475ba378c32a0c180bd0
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04968798

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