Sulfuric Acid → HCID 19699091、化合物

HRID 2255955ノート

反応式

HRID 2255955 の反応式
[O:1]=[C:2]1[C:7]2[C:8]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][O:10][C:6]=2[CH2:5][CH2:4][CH2:3]1.[N-:15]=[N+]=[N-].[Na+].S(=O)(=O)(O)O.[NH4+].[OH-]>C(Cl)(Cl)Cl.O>[O:1]=[C:2]1[NH:15][C:7]2[C:8]([C:11]([O:13][CH3:14])=[O:12])=[CH:9][O:10][C:6]=2[CH2:5][CH2:4][CH2:3]1

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 14923Ammonium HydroxideHCID 33557Sodium AzideHCID 11499367Methyl 4-oxo-4,5,6,7-tetrahydro-1-benzofuran-3-carboxylate

生成物 1

HCID 19699091HCID 19699091、化合物収率 92.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

To a mixture of 1.0 g of methyl 4,5,6,7-tetrahydro-4-oxo-3-benzofurancarboxylate and 502 mg of sodium azide in 5 ml of chloroform is added dropwise at 32°-36° C. under argon 1.4 ml of sulfuric acid. The reaction mixture is stirred at room temperature for 24 hours. The reaction mixture is diluted with 14 ml of water and rendered alkaline with NH4OH and extracted with chloroform. The separated organic layer is washed with water, brine and dried with Na2SO4 and concentrated in vacuo to give 1.0 g of the desired product as a white solid.

後処理

  1. extractionextracted with chloroform
  2. washThe separated organic layer is washed with water, brine
  3. dry with materialdried with Na2SO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-67d5e0c5937c4d3bba243782bbcad65c
出典データセット
uspto-grants-1997_08
特許番号
US05654297

反応ノート

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