Borohydride → 3,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-9-ol

HRID 459912

反応式

HRID 459912 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:13])[CH2:9][CH2:8]2)[O:4][CH2:3]1.[BH4-]>CO>[CH3:1][C:2]1([CH3:14])[CH2:3][O:4][C:5]2([CH2:8][CH2:9][CH:10]([OH:13])[CH2:11][CH2:12]2)[O:6][CH2:7]1

参加物

4

反応物 2

HCID 28123BorohydrideHCID 5879683,3-Dimethyl-1,5-dioxaspiro(5.5)undecan-9-one

生成物 1

HCID 124700963,3-Dimethyl-1,5-dioxaspiro[5.5]undecan-9-ol

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Combine 3,3-dimethyl-1,5-dioxa-spiro[5.5]undecan-9-one (Aldrich, 750 mg, 3.78 mmol) with polymer-supported borohydride (Aldrich, 3026 mg, 7.56 mmol) in methanol (30 mL). Shake by rotation the resulting mixture overnight. Filter the reaction mixture and concentrate the filtrate. Wash the residue with hydrochloric acid 0.1M and extract with EtOAc. Dry the organic layer over sodium sulfate, filter and concentrate.

後処理

  1. customthe resulting mixture overnight
  2. filtrationFilter the reaction mixture
  3. concentrationconcentrate the filtrate
  4. washWash the residue with hydrochloric acid 0.1M
  5. extractionextract with EtOAc
  6. dry with materialDry the organic layer over sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate

出典と根拠

ORDレコード
ord-bfbde5ec2c73434e868e22d83e2af1ee
出典データセット
uspto-grants-2007_03
特許番号
US07196100B2

関連ノート

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