2-Methyl-1,6-dioxaspiro[4.4]nonane-2-carbaldehyde → (2-Methyl-1,6-dioxaspiro[4.4]nonan-2-yl)methanol

HRID 647754ノート

反応式

HRID 647754 の反応式
[CH3:1][C:2]1([CH:11]=[O:12])[CH2:6][CH2:5][C:4]2([CH2:10][CH2:9][CH2:8][O:7]2)[O:3]1>O1CCCC1>[CH3:1][C:2]1([CH2:11][OH:12])[CH2:6][CH2:5][C:4]2([CH2:10][CH2:9][CH2:8][O:7]2)[O:3]1

参加物

3

反応物 1

HCID 132371812-Methyl-1,6-dioxaspiro[4.4]nonane-2-carbaldehyde

生成物 1

HCID 13237169(2-Methyl-1,6-dioxaspiro[4.4]nonan-2-yl)methanol収率 83.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 1.70 g of 2-methyl-1,6-dioxaspiro[4.4]nonane-2-carboxaldehyde in tetrahydrofuran was hydrogenated at 60 p.s.i. and 20° C. for 5 hours in the presence of 1.0 g triethylamine promoter and Raney nickel, that had been rinsed in tetrahydrofuran. When all of the starting material had disappeared, the mixture was treated with magnesium sulfate and filtered. Distillation of the filtrate gave 1.43 g of the desired product as a colorless liquid, b.p. 65°-70° C. (1 torr.).

後処理

  1. washand 20° C. for 5 hours in the presence of 1.0 g triethylamine promoter and Raney nickel, that had been rinsed in tetrahydrofuran
  2. additionthe mixture was treated with magnesium sulfate
  3. filtrationfiltered
  4. distillationDistillation of the filtrate

出典と根拠

ORDレコード
ord-c6cbff53a17447c4b2e97852d06bf064
出典データセット
uspto-grants-1983_10
特許番号
US04410354

反応ノート

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