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ChemicalBook CAS DataBase List 1,4-dioxaspiro[4.4]nonan-7-ylmethanol

1,4-dioxaspiro[4.4]nonan-7-ylmethanol synthesis

4synthesis methods
77250-34-1 Synthesis
methyl 1,4-dioxaspiro[4.4]nonane-7-carboxylate

77250-34-1
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$417.00/1g

1,4-dioxaspiro[4.4]nonan-7-ylmethanol

65005-20-1
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Yield:65005-20-1 88%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran at -10 - 25; for 3 h;Inert atmosphere;

Steps:

10.2 Second Step
(1,4-dioxa-spiro [4.4] nonane-7-yl) -methanol

1,4-dioxa-spiro [4.4] nonane-7-carboxylate (1.00g, 10.7mmol) was dissolved in dry tetrahydrofuran (30 mL) in nitrogen atmosphere, -10°C was slowly added lithium aluminum tetrahydride (531mg, 13.9mmol). The reaction solution was gradually raised to 25°C, stirred for 3 hours. To the reaction mixture were added successively water (0.5mL), 15% sodium hydroxide solution (0.5mL), water (1.5mL). Insolubles were removed by filtration, the filtrate was concentrated under reduced pressure to give (1,4-Dioxa-spiro [4.4] nonane-7-yl) - methanol (1.5mg, yellow oil). Yield: 88%.

References:

CN105566324,2016,A Location in patent:Paragraph 0232; 0236; 0237; 0238