Hydrochloric Acid → 5-azidopentanoic Acid

HRID 386422ノート

反応式

HRID 386422 の反応式
[N:1]([CH2:4][CH2:5][CH2:6][CH2:7][C:8]([O:10]CC)=[O:9])=[N+:2]=[N-:3].CN(C)C=O.[OH-].[Li+].Cl>O>[N:1]([CH2:4][CH2:5][CH2:6][CH2:7][C:8]([OH:10])=[O:9])=[N+:2]=[N-:3]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 6228DimethylformamideHCID 123821765-Azidopentanoic acid ethyl ester

生成物 1

HCID 111161715-azidopentanoic Acid収率 99%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
25 °C

実験手順

To ethyl 5-azidovalerate (1.6 g; 10 mmol; Example 2.1) in 5 ml-dimethylformamide, was added lithium hydroxide (1.0 g; 20 mmol; Fisher) in 5 ml water, and the reaction mixture was stirred 12 h at 25° C. The reaction mixture was adjusted to pH ˜4 by addition of 1 N HCl and was extracted with 100 ml diethyl ether. The resulting organic layer was washed with water (100 ml) and brine (100 ml), dried over sodium sulfate, and dried in vacuo. Yield: 1.4 g (9.8 mmol, 99% yield).

後処理

  1. extractionwas extracted with 100 ml diethyl ether
  2. washThe resulting organic layer was washed with water (100 ml) and brine (100 ml)
  3. dry with materialdried over sodium sulfate
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-5ca6025cb0c84ab8afc1e58f3fb6d681
出典データセット
uspto-grants-2013_02
特許番号
US08372839B2

反応ノート

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