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

HRID 1458894ノート

反応式

HRID 1458894 の反応式
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

参加物

3

反応物 1

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

生成物 1

HCID 131720990HCID 131720990、化合物収率 87%

試薬・触媒・溶媒 1

HCID 10942334Sodium Methoxide溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-0d7bbddd8420494d8a3585512e757c26
出典データセット
uspto-grants-1998_12
特許番号
US05852038

反応ノート

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