Ammonia → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine

HRID 342476

反応式

HRID 342476 の反応式
[CH3:1][C:2]1([CH3:14])[CH2:7][O:6][C:5]2([CH2:12][CH2:11][C:10](=O)[CH2:9][CH2:8]2)[O:4][CH2:3]1.[NH3:15].[H][H]>CO.[Ni]>[CH3:1][C:2]1([CH3:14])[CH2:7][O:6][C:5]2([CH2:12][CH2:11][CH:10]([NH2:15])[CH2:9][CH2:8]2)[O:4][CH2:3]1

参加物

6

反応物 3

HCID 222AmmoniaHCID 5879683,3-Dimethyl-1,5-dioxaspiro(5.5)undecan-9-oneHCID 178418361HCID 178418361、化合物

生成物 1

HCID 599703173,3-Dimethyl-1,5-dioxaspiro[5.5]undec-9-ylamine

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

A solution of 20.0 g (0.1 mol) of 3,3-dimethyl-1,5-dioxaspiro[5.5]undecan-9-one in 250 ml of methanol which contained 38 g of ammonia was hydrogenated at 100° C. and a hydrogen pressure of 100 bar in the presence of 3 g of Raney nickel. The catalyst was filtered off and the solvent was stripped off in vacuo. The crude product was purified by means of a thin film evaporator (140° C./0.8 bar). This gave 16 g (80% of theory) of distillate which solidified upon standing.

後処理

  1. customwas hydrogenated at 100° C.
  2. filtrationThe catalyst was filtered off
  3. customThe crude product was purified by means of a thin film evaporator (140° C./0.8 bar)

出典と根拠

ORDレコード
ord-1f876b8756394ccf8b294e4ac8acb593
出典データセット
uspto-grants-1999_01
特許番号
US05859009

関連ノート

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