Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate → 2,5-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

HRID 345815

反応式

HRID 345815 の反応式
[CH3:1][N:2]1[O:9][CH2:8][C:7]2([CH3:10])[CH:3]1[CH2:4][N:5](C(OCC)=O)[CH2:6]2>O>[CH3:1][N:2]1[O:9][CH2:8][C:7]2([CH3:10])[CH:3]1[CH2:4][NH:5][CH2:6]2

参加物

3

反応物 1

HCID 15070010Ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate

生成物 1

HCID 150700112,5-Dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

13 g (60.6 mmol) of ethyl 2,5-dimethyl-3-oxa-2,7-diazabicyclo[3.3.0]octane-7-carboxylate are heated under reflux with 33 g of Ba(OH)2.8H2O in 330 ml of water overnight. The BaCO3 is filtered off with suction, K2CO3 is added to the filtrate, the solid is filtered off with suction again and the filtrate is extracted ten times with 100 ml of CHCl3 each time. The extracts are dried over K2CO3 and concentrated and the residue is distilled.

後処理

  1. filtrationThe BaCO3 is filtered off with suction, K2CO3
  2. additionis added to the filtrate
  3. filtrationthe solid is filtered off with suction again
  4. extractionthe filtrate is extracted ten times with 100 ml of CHCl3 each time
  5. dry with materialThe extracts are dried over K2CO3
  6. concentrationconcentrated
  7. distillationthe residue is distilled

出典と根拠

ORDレコード
ord-8a25500a2fdf4cf981d2acc05cfb34ce
出典データセット
uspto-grants-1991_10
特許番号
US05059597

関連ノート

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