Cyclohexylamine → HCID 10403249、化合物

HRID 1744779ノート

反応式

HRID 1744779 の反応式
[N+:1]([CH2:4][C@:5]1([CH2:12][C:13]([OH:15])=[O:14])[CH2:11][C@@H:10]2[C@H:6]1[CH2:7][CH2:8][CH2:9]2)([O-:3])=[O:2].C1(N)CCCCC1>C(OCC)(=O)C>[CH:4]1([NH2:1])[CH2:5][CH2:11][CH2:10][CH2:6][CH2:7]1.[N+:1]([CH2:4][C@:5]1([CH2:12][C:13]([OH:15])=[O:14])[CH2:11][C@@H:10]2[C@H:6]1[CH2:7][CH2:8][CH2:9]2)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 10255676HCID 10255676、化合物

生成物 1

HCID 10403249HCID 10403249、化合物収率 177.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
40 °C

実験手順

A solution of nitro acid of Example 8 (928 g; 4.35 mol) in ethyl acetate (9.6 L) was dried by atmospheric azeotropic distillation at constant volume. After cooling the solution to 40° C., cyclohexylamine (423 g; 4.26 mol) was added over 15 minutes. The resultant slurry was cooled to 20° C. over 4 hours and left to stir for 13 hours at 20° C. The solid was collected by filtration and the damp filter cake washed with ethyl acetate (1.3 L). The isolated solid was then dried in vacuo at 30° C. for 18 hours to give the title compound as a white solid (1.205 Kg) in 91% yield.

後処理

  1. temperatureThe resultant slurry was cooled to 20° C. over 4 hours
  2. waitleft
  3. filtrationThe solid was collected by filtration
  4. washthe damp filter cake washed with ethyl acetate (1.3 L)
  5. customThe isolated solid was then dried in vacuo at 30° C. for 18 hours

出典と根拠

ORDレコード
ord-dc9e379f47a846cab451df7e49f63a6a
出典データセット
uspto-grants-2006_03
特許番号
US07018818B2

反応ノート

読み込み中…