4-Methylmorpholine → HCID 59140422、化合物

HRID 1881396ノート

反応式

HRID 1881396 の反応式
CN1CCOCC1.[CH3:8][C:9]([CH3:18])([CH2:16][CH3:17])[CH2:10][C:11]1[N:12]=[CH:13][NH:14][CH:15]=1.[CH3:19][N:20]([CH3:25])[S:21](Cl)(=[O:23])=[O:22]>C(COC)OC>[CH3:8][C:9]([CH3:18])([CH2:16][CH3:17])[CH2:10][C:11]1[N:12]=[CH:13][N:14]([S:21]([N:20]([CH3:25])[CH3:19])(=[O:23])=[O:22])[CH:15]=1

参加物

5

反応物 3

HCID 79724-Methylmorpholine2 回HCID 83372Dimethylsulphamoyl chloride2 回HCID 178442466HCID 178442466、化合物

生成物 1

HCID 59140422HCID 59140422、化合物

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
40 °C

実験手順

N-methylmorpholine (54 mL, 0.48 mol) was added to a solution of 4-(2,2-dimethylbutyl)-1H-imidazole (36 g, 0.24 mol) in dimethoxyethane (360 mL). After warming to 40° C., N,N-dimethylsulfamoyl chloride (38 mL, 0.36 mol) was added over 15 min. After stirring at 40° C. for 2 h, N-methylmorpholine (11 mL) and N,N-dimethylsulfamoyl chloride (8 mL) were added. After stirring for an additional 2 h the reaction mixture was cooled and filtered rinsing with ether. The filtrate was extracted with ether. The combined organic extracts were washed with brine, dried (magnesium sulfate), filtered, concentrated in vacuo. Chromatography over silica afforded the title compound.

後処理

  1. stirringAfter stirring for an additional 2 h the reaction mixture
  2. temperaturewas cooled
  3. filtrationfiltered
  4. washrinsing with ether
  5. extractionThe filtrate was extracted with ether
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried (magnesium sulfate)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f57393107af74bda8f035b0e5ffa16ea
出典データセット
uspto-grants-2012_11
特許番号
US08318767B2

反応ノート

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