N,N-Diethyl-6-diphenylmethyl-5,5-ethylenedioxy-1-azabicyclo-[2.2.2]octane-3-carboxamide → HCID 131720990, 화합물

HRID 1458894노트

반응식

HRID 1458894 반응식
C([N:3](CC)[C:4]([CH:6]1[CH:11]2[CH2:12][CH2:13][N:8]([CH:9](C(C3C=CC=CC=3)C3C=CC=CC=3)[C:10]32[O:17][CH2:16][CH2:15][O:14]3)[CH2:7]1)=[O:5])C>C[O-].[Na+]>[CH2:15]1[CH2:16][O:17][C:10]2([CH2:9][N:8]3[CH2:13][CH2:12][CH:11]2[CH:6]([C:4]([NH2:3])=[O:5])[CH2:7]3)[O:14]1

참가 물질

3

반응물 1

HCID 53633468N,N-Diethyl-6-diphenylmethyl-5,5-ethylenedioxy-1-azabicyclo-[2.2.2]octane-3-carboxamide

생성물 1

HCID 131720990HCID 131720990, 화합물수율 87%

시약·촉매·용매 1

HCID 10942334Sodium Methoxide용매

실험 절차

A suspension of 21 (9.8 g, 22 mmol) in sodium methoxide (28% in MeOH; 400 g) was heated at reflux temperature for 9 hours. The resulting solution was poured on ice (300 ml) and extracted with CH2Cl2 (150 ml) three times. The combined extracts were dried over sodium sulfate (Na2SO4) and concentrated. The clude was purified by recrystallization from ethanol (EtOH) to give 22 (1:4 mixture at 6-position ; 8.4 9, 19 mmol, 87%).

후처리

  1. temperaturewas heated
  2. temperatureat reflux temperature for 9 hours
  3. additionThe resulting solution was poured on ice (300 ml)
  4. extractionextracted with CH2Cl2 (150 ml) three times
  5. dry with materialThe combined extracts were dried over sodium sulfate (Na2SO4)
  6. concentrationconcentrated
  7. customThe clude was purified by recrystallization from ethanol (EtOH)

출처 및 근거

ORD 기록
ord-0d7bbddd8420494d8a3585512e757c26
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05852038

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