Diisopropylethylamine → HCID 18519986, 화합물

HRID 1936730노트

반응식

HRID 1936730 반응식
C(N(CC)C(C)C)(C)C.Cl.[CH3:11][O:12][NH2:13].[C:14]1(=[O:21])[CH:20]=[CH:19][CH2:18][CH2:17][CH:16]=[CH:15]1>C(O)(C)C>[CH3:11][O:12][N:13]1[CH:19]2[CH2:18][CH2:17][CH:16]1[CH2:15][C:14](=[O:21])[CH2:20]2

참가 물질

5

반응물 3

HCID 81531Diisopropylethylamine2회HCID 521874O-Methylhydroxylamine hydrochlorideHCID 109204632,6-Cycloheptadien-1-one

생성물 1

HCID 18519986HCID 18519986, 화합물수율 20%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

N,N-Diisoproylethylamine (14.5 ml) was added dropwise to a stirred suspension of O-methylhydroxylamine hydrochloride (2.32 g) in isopropyl alcohol (25 ml). After 30 minutes cyclohepta-2,6-dienone (3.0 g) in isopropyl alcohol (5 ml) was added dropwise. After 24 hours N,N-diisopropylethylamine (4.9 ml) was added. After 6 hours the mixture was allowed to stand at room temperature overnight. The mixture was evaporated under reduced pressure, diethyl ether added and the resulting mixture extracted with 2M hydrochloric acid (x3). The combined aqueous fractions were washed with diethyl ether (x3), neutralised with sodium hydroxide and extracted with diethyl ether (x3). The combined extracts were washed with brine, dried (MgSO4) and evaporated under reduced pressure. Kugelrohr distillation gave 8-methoxy-8-azabicyclo[3.2.1]octan-3-one (0.86 g).

후처리

  1. waitto stand at room temperature overnight
  2. customThe mixture was evaporated under reduced pressure, diethyl ether
  3. additionadded
  4. extractionthe resulting mixture extracted with 2M hydrochloric acid (x3)
  5. washThe combined aqueous fractions were washed with diethyl ether (x3)
  6. extractionextracted with diethyl ether (x3)
  7. washThe combined extracts were washed with brine
  8. dry with materialdried (MgSO4)
  9. customevaporated under reduced pressure
  10. distillationKugelrohr distillation

출처 및 근거

ORD 기록
ord-4c8e9ae7457343029b6921c0978c78ca
출처 데이터셋
uspto-grants-2002_05
특허 번호
US06391883B1

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