Water → N-{2-[4(3,4-dichlorophenoxy)-1-piperidinyl]ethyl}-3-methoxybenzamide

HRID 968765ノート

反応式

HRID 968765 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.[CH3:26][O:27][C:28]1[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=1)[C:31](Cl)=[O:32].O>C1COCC1>[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:31](=[O:32])[C:30]2[CH:34]=[CH:35][CH:36]=[C:28]([O:27][CH3:26])[CH:29]=2)[CH2:10][CH2:11]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 74374m-Anisoyl chlorideHCID 113582094-(3,4-Dichlorophenoxy)-1-piperidineethanamine

生成物 1

HCID 9910169N-{2-[4(3,4-dichlorophenoxy)-1-piperidinyl]ethyl}-3-methoxybenzamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The product from Example 3, Step b (2.00 g) was dissolved in TBF (100 ml) and triethylamine (2.10 g) added. The solution was then cooled with stirring to 0° C. and to it 3-methoxybenzoyl chloride was added dropwise as a solution in THF (10 ml). Reaction was left to warm to room temp and left for 24 hours then water was added and the organics extracted into ethyl acetate. The combined organics were dried with MgSO4 and the solvent removed by evaporation. The crude product was purified by flash chromatography to leave the sub-title product as a pale yellow oil (1.38 g).

後処理

  1. temperatureThe solution was then cooled
  2. customReaction
  3. waitwas left
  4. extractionthe organics extracted into ethyl acetate
  5. dry with materialThe combined organics were dried with MgSO4
  6. customthe solvent removed by evaporation
  7. customThe crude product was purified by flash chromatography

出典と根拠

ORDレコード
ord-4ea4457e9599494bbd3bb90bc955551f
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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