Ethanol → HCID 69522441、化合物

HRID 968771ノート

反応式

HRID 968771 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 69522441HCID 69522441、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3ddb5fc434d641dcb08a4eb1c88b3666
出典データセット
uspto-grants-2007_12
特許番号
US07304077B2

反応ノート

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