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

HRID 647754노트

반응식

HRID 647754 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-c6cbff53a17447c4b2e97852d06bf064
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410354

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