Sodium Azide → 8-Azido-1,4-dioxaspiro[4.5]decane

HRID 1190061

反応式

HRID 1190061 の反応式
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8](OS(C)(=O)=O)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[N-:16]=[N+:17]=[N-:18].[Na+]>CN(C=O)C.[Cl-].[Na+].O>[N:16]([CH:8]1[CH2:9][CH2:10][C:5]2([O:4][CH2:3][CH2:2][O:1]2)[CH2:6][CH2:7]1)=[N+:17]=[N-:18]

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 149667411,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate

生成物 1

HCID 574240948-Azido-1,4-dioxaspiro[4.5]decane収率 100.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 57417360Sodium chloride; water溶媒

反応条件

温度
100 °C

実験手順

A mixture of methanesulfonic acid 1,4-dioxa-spiro[4.5]dec-8-yl ester (2.80 g, 11.9 mmol) and sodium azide (3.86 g, 59.3 mmol) in 50 mL of dry DMF was stirred for 20 h at 100° C. under nitrogen. The final mixture was cooled to room temperature dilute with brine and extracted with three portions of ether. The organic portions were combined, dried over Na2SO4 and concentrated to give 8-azido-1,4-dioxa-spiro[4.5]decane (2.2 g, 100%).

後処理

  1. extractionextracted with three portions of ether
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-cb31b2c05cf44bd1aaaeb70cfa80f4cb
出典データセット
uspto-grants-2014_03
特許番号
US08674118B2

関連ノート

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