Ethyl chloroformate → HCID 13282864、化合物

HRID 1388181ノート

反応式

HRID 1388181 の反応式
[CH2:1]([O:3][C:4]([N:6]1[C:10]2([CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH:9]([NH2:16])[CH2:8][CH2:7]1)=[O:5])[CH3:2].C([O-])(O)=O.[Na+].Cl[C:23]([O:25][CH2:26][CH3:27])=[O:24]>C(Cl)(Cl)Cl>[CH2:1]([O:3][C:4]([N:6]1[C:10]2([CH2:15][CH2:14][CH2:13][CH2:12][CH2:11]2)[CH:9]([NH:16][C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 10928Ethyl chloroformateHCID 516892Sodium BicarbonateHCID 13282855Ethyl 4-amino-1-azaspiro[4.5]decane-1-carboxylate

生成物 1

HCID 13282864HCID 13282864、化合物収率 79.8%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a stirring suspension of 5.7 g of 1-ethoxycarbonyl-4-amino-1-azaspiro[4.5]decane of Example 1e and 7. g of NaHCO3 in 100 ml of CHCl3 was added in a dropwise fashion 3.8 g of ethyl chloroformate. The mixture was refluxed for 4 hours, cooled to room temperature, filtered, washed with water, 3 N-HCl, saturated sodium bicarbonate solution and saturated NaCl solution, dried over Na2SO4 and then evaporated to give 6 g of 1-ethoxycarbonyl-4-(ethoxycarbonylamino)-1-azaspiro[4.5]decane.

後処理

  1. temperatureThe mixture was refluxed for 4 hours
  2. filtrationfiltered
  3. washwashed with water, 3 N-HCl, saturated sodium bicarbonate solution and saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. customevaporated

出典と根拠

ORDレコード
ord-9d133adcc7154c5a9821c2569b620d65
出典データセット
uspto-grants-1984_02
特許番号
US04430335

反応ノート

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