Sulfamic Acid → 2-(4-Iodophenyl)propanoic acid

HRID 904232

반응식

HRID 904232 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:11])[CH:9]=[O:10])=[CH:4][CH:3]=1.S(=O)(=O)([OH:14])N.Cl([O-])=O.[Na+].S([O-])(O)=O.[Na+]>C(Cl)CCl.O>[I:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]([CH3:11])[C:9]([OH:14])=[O:10])=[CH:6][CH:7]=1

참가 물질

7

반응물 4

HCID 5987Sulfamic AcidHCID 233338292-(4-Iodophenyl)propanalHCID 23665763Sodium BisulfiteHCID 23668197Sodium Chlorite

생성물 1

HCID 152255732-(4-Iodophenyl)propanoic acid수율 94.2%

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 962Water용매2회

실험 절차

To a solution of 34 g of 2-(4-iodophenyl)propionaldehyde in 100 ml of ethylene chloride was added a solution of 16.5 g of sulfamic acid in 85 ml of water. To the mixture was added dropwise with stirring a solution of 15.2 g of sodium chlorite in 22 ml of water, while maintaining the temperature at 10° to 15° C. After stirring for 10 minutes, about 15 g of sodium hydrogensulfite was added in small portions to the mixture. The organic layer was separated, washed with water, and mixed with 150 ml of 1 N sodium hydroxide solution. The aqueous layer was separated and adjusted to pH 3.0 with 6 N hydrochloric acid to precipitate white crystals. The crystals were collected by filtration, washed with water, and dried to obtain 34 g (94% yield) of 2-(4-iodophenyl)propionic acid.

후처리

  1. additionTo the mixture was added dropwise
  2. temperaturewhile maintaining the temperature at 10° to 15° C
  3. customThe organic layer was separated
  4. washwashed with water
  5. additionmixed with 150 ml of 1 N sodium hydroxide solution
  6. customThe aqueous layer was separated
  7. customto precipitate white crystals
  8. filtrationThe crystals were collected by filtration
  9. washwashed with water
  10. customdried

출처 및 근거

ORD 기록
ord-df16276f14824d189c533c6068590210
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04230719

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