Ethanol → HCID 69522441, 화합물

HRID 968771노트

반응식

HRID 968771 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][C:17]=1[Cl:18])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][NH2:14])[CH2:8][CH2:7]1.C(N(CC)CC)C.[OH2:26].[NH2:27][NH2:28].[CH2:29]([OH:31])[CH3:30]>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]([CH:15]=[CH:16][C:17]=1[Cl:18])[O:5][CH:6]1[CH2:7][CH2:8][N:9]([CH2:12][CH2:13][NH:14][C:30](=[O:26])[C:29]([NH:27][NH2:28])=[O:31])[CH2:10][CH2:11]1

참가 물질

6

반응물 4

HCID 702EthanolHCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 113582094-(3,4-Dichlorophenoxy)-1-piperidineethanamine

생성물 1

HCID 69522441HCID 69522441, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of the product of Example 3, Step b (0.85 g) and triethylamine (0.82 ml) at RT in dichloromethane (20 ml) was added methyl oxalyl chloride (0.30 ml) dropwise over 10 minutes. The reaction mixture was partitioned between water (20 ml) and dichloromethane (20 ml). The organic phase was separated and dried with MgSO4. Evaporation under reduced pressure gave an oil which was dissolved in ethanol (10 ml) at RT and treated with hydrazine hydrate (1 ml) The reaction mixture was stirred at reflux for 24 hours, filtered and the filtrate evaporated under reduced pressure to leave an oil. Purification by flash chromatography (dichloromethane:methanol 90:10)gave the sub-title compound as a white solid (0.18 g).

후처리

  1. customThe reaction mixture was partitioned between water (20 ml) and dichloromethane (20 ml)
  2. customThe organic phase was separated
  3. dry with materialdried with MgSO4
  4. customEvaporation under reduced pressure
  5. customgave an oil which
  6. temperatureat reflux for 24 hours
  7. filtrationfiltered
  8. customthe filtrate evaporated under reduced pressure
  9. customto leave an oil
  10. customPurification by flash chromatography (dichloromethane

출처 및 근거

ORD 기록
ord-3ddb5fc434d641dcb08a4eb1c88b3666
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07304077B2

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