Ethyl chloroformate → HCID 13282864, 화합물

HRID 1388181노트

반응식

HRID 1388181 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 13282864HCID 13282864, 화합물수율 79.8%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d133adcc7154c5a9821c2569b620d65
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04430335

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