Water → HCID 64842474、化合物

HRID 2360713ノート

反応式

HRID 2360713 の反応式
[CH2:1]([N:8]1[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][C:14](=O)[C:9]21[CH2:13][CH2:12][CH2:11][CH2:10]2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].Cl[Si](C)(C)C.O>C1COCC1>[CH2:1]([N:8]1[CH2:17][C:16]([CH3:19])([CH3:18])[NH:15][CH2:14][C:9]21[CH2:10][CH2:11][CH2:12][CH2:13]2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 6397ChlorotrimethylsilaneHCID 21226445Aluminium lithium hydrideHCID 866803356-Benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one

生成物 1

HCID 64842474HCID 64842474、化合物収率 93%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

反応条件

温度
55 °C

実験手順

Under Argon atmosphere to a solution of 10.78 g of 6-benzyl-8,8-dimethyl-6,9-diaza-spiro[4.5]decan-10-one in 160 ml of THF 33 ml of a 2.4 M solution of lithium aluminium hydride in THF were slowly added. The reaction was heated to 55° C., and 5 ml of chlorotrimethylsilane were added dropwise. The reaction was kept at 55-60° C. for 2.5 h and then cooled to 0° C. 16 ml of water were added dropwise, and THF was added. The mixture was filtered by suction over celite and the filtrate was concentrated in vacuo. The product was precipitated by treatment with methyl tert-butyl ether. 9.47 g (93%) of the title compound were obtained.

後処理

  1. temperaturecooled to 0° C
  2. filtrationThe mixture was filtered by suction over celite
  3. concentrationthe filtrate was concentrated in vacuo
  4. customThe product was precipitated by treatment with methyl tert-butyl ether

出典と根拠

ORDレコード
ord-d656a166e42446d19edf28ab71225e61
出典データセット
uspto-grants-2014_04
特許番号
US08686150B2

反応ノート

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