Sulfamic Acid → 7-Methoxy-2-methylbenzo[b]furan-4-carboxylic acid

HRID 1091831노트

반응식

HRID 1091831 반응식
[CH3:1][O:2][C:3]1[C:8]2[O:9][C:10]([CH3:12])=[CH:11][C:7]=2[C:6]([CH:13]=[O:14])=[CH:5][CH:4]=1.S(=O)(=O)([OH:17])N.Cl([O-])=O.[Na+]>CC(C)=O.O>[CH3:1][O:2][C:3]1[C:8]2[O:9][C:10]([CH3:12])=[CH:11][C:7]=2[C:6]([C:13]([OH:17])=[O:14])=[CH:5][CH:4]=1

참가 물질

6

반응물 3

HCID 5987Sulfamic AcidHCID 110415447-Methoxy-2-methyl-1-benzofuran-4-carbaldehydeHCID 23668197Sodium Chlorite

생성물 1

HCID 220095237-Methoxy-2-methylbenzo[b]furan-4-carboxylic acid

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매

실험 절차

To a well stirred solution of 7-methoxy-2-methylbenzo[b]furan-4-carboxaldehyde (from step 3) (4.0 g, 21.05 mmol) in acetone (40.0 mL) was added a solution of sulphamic acid (2.4 g, 25.26 mmol) in water (10.0 mL) followed by addition of a solution of sodium chlorite (2.8 g, 31.57 mmol) at 5-10° C. Ice cold water (250 mL) was added to reaction mixture and the product separated was filtered and dried at 60-70° C. to give intermediate-4 (3.2 g) as white solid.

후처리

  1. customthe product separated
  2. filtrationwas filtered
  3. customdried at 60-70° C.
  4. customto give intermediate-4 (3.2 g) as white solid

출처 및 근거

ORD 기록
ord-283717dce906448dab67a3af90df7297
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129401B2

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