HCID 13282864, 화합물 → N,1-Dimethyl-1-azaspiro[4.5]decan-4-amine

HRID 1388182노트

반응식

HRID 1388182 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].C(O[C:10]([N:12]1[C:16]2([CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)[CH:15]([NH:22][C:23](OCC)=O)[CH2:14][CH2:13]1)=O)C>C1COCC1>[CH3:10][N:12]1[C:16]2([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21]2)[CH:15]([NH:22][CH3:23])[CH2:14][CH2:13]1

참가 물질

4

반응물 2

HCID 13282864HCID 13282864, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 13282865N,1-Dimethyl-1-azaspiro[4.5]decan-4-amine수율 55.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirring solution of 2.4 g of lithium aluminum hydride (LAH) in 200 ml of THF was added in a dropwise manner 6.5 g of 1-ethoxycarbonyl-4-(ethoxycarbonylamino)-1-azaspiro[4.5]decane of Example 10 in 70 ml of THF. The resultant mixture was refluxed overnight, and then kept at room temperature for 48 hours. The excess LAH was destroyed with water, and the resultant mixture was filtered, washed with ether and then evaporated and then distilled at 55° C., 0.1 mm to yield 2.2 g of 1-methyl-4-methylamino-1-azaspiro[4.5]decane.

후처리

  1. customThe excess LAH was destroyed with water
  2. filtrationthe resultant mixture was filtered
  3. washwashed with ether
  4. customevaporated
  5. distillationdistilled at 55° C.

출처 및 근거

ORD 기록
ord-4d47cd6b32f94618bd9930abdf570d09
출처 데이터셋
uspto-grants-1984_02
특허 번호
US04430335

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