Sulfuric Acid → HCID 19699091, 화합물

HRID 2255955노트

반응식

HRID 2255955 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 19699091HCID 19699091, 화합물수율 92.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-67d5e0c5937c4d3bba243782bbcad65c
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05654297

반응 노트

불러오는 중…