HCID 13282864、化合物 → N,1-Dimethyl-1-azaspiro[4.5]decan-4-amine

HRID 1388182ノート

反応式

HRID 1388182 の反応式
[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

参加物

4

反応物 2

HCID 13282864HCID 13282864、化合物HCID 21226445Aluminium lithium hydride

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-4d47cd6b32f94618bd9930abdf570d09
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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