Sodium borohydride → HCID 23003686、化合物

HRID 396312ノート

反応式

HRID 396312 の反応式
[BH4-].[Na+].[CH2:3]([N:10]1[CH2:15][CH2:14][C:13](=[O:16])[C:12]([CH2:18][CH3:19])([CH3:17])[CH2:11]1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>CO>[CH2:3]([N:10]1[CH2:15][CH2:14][CH:13]([OH:16])[C:12]([CH2:18][CH3:19])([CH3:17])[CH2:11]1)[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 22278904HCID 22278904、化合物

生成物 1

HCID 23003686HCID 23003686、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium borohydride (0.3 g, 9.0 mmole) was added to the stirred solution of the 1-benzyl-3-ethyl-3-methylpiperid-4-one (1.5 g, 6.5 mmole) in methanol (20 ml) at 0-5° C. over a period of 5 min, and stirring was continued for 2 hr at ambient temperature. The reaction mixture was concentrated to dryness, triturated with water (20 ml) and extracted with ethyl acetate (2×50 ml). The extract was dried over sodium sulphate and concentrated to dryness to furnish 1-benzyl-3-ethyl-4-hydroxy-3-methylpiperidine product as oil, which was used as such in the next step. Yield 1.1 g (74%), C15H23NO, m/z 234 (M+1).

後処理

  1. concentrationThe reaction mixture was concentrated to dryness
  2. customtriturated with water (20 ml)
  3. extractionextracted with ethyl acetate (2×50 ml)
  4. dry with materialThe extract was dried over sodium sulphate
  5. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-5535690c20dc438698ef8700252ad955
出典データセット
uspto-grants-2003_08
特許番号
US06608078B2

反応ノート

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