Cyclohexylamine → HCID 10403249, 화합물

HRID 1744779노트

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HRID 1744779 반응식
[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]

참가 물질

4

반응물 2

HCID 7965CyclohexylamineHCID 10255676HCID 10255676, 화합물

생성물 1

HCID 10403249HCID 10403249, 화합물수율 177.3%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

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온도
40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dc9e379f47a846cab451df7e49f63a6a
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07018818B2

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