Water → 2-(1,2-Benzoxazol-3-yl)acetic acid

HRID 855934

반응식

HRID 855934 반응식
S(O)(O)(=O)=O.[NH2:6][OH:7].[OH2:8].[OH-:9].[Na+].O[C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)O[C:14](=O)[CH:13]=1>O.O.[Na+].[Na+].C(N(CC(O)=O)CC(O)=O)CN(CC([O-])=O)CC([O-])=O.ClCCCl>[O:7]1[C:20]2[CH:19]=[CH:18][CH:17]=[CH:16][C:21]=2[C:12]([CH2:13][C:14]([OH:9])=[O:8])=[N:6]1

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 159255Hydroxylamine, sulfate (1:1)HCID 546829304-Hydroxycoumarin

생성물 1

HCID 3017292-(1,2-Benzoxazol-3-yl)acetic acid

시약·촉매·용매 2

HCID 44120005Edta disodium촉매HCID 111,2-Dichloroethane용매

실험 절차

A mixture of hydroxylamine sulfate (344.0 g), water (904 ml) and a 25% aqueous sodium hydroxide solution (456 ml) is stirred, and thereto are added 4-hydroxycoumarin (168.0 g) and ethylenediaminetetraacetic acid disodium salt dihydrate (3.2 g), and the mixture is stirred with heating at 84° C.-86° C. for 4 hours. The reaction mixture is cooled, and thereto is added 1,2-dichloroethane (240 ml). The mixture is stirred, and the aqueous layer is collected. The pH value of the aqueous layer is adjusted to pH 1-2 with 25% sulfuric acid, and the precipitated crystals are collected by filtration, washed with water, and dried with air at 60° C. for 15 hours to give 1,2-benzisoxazole-3-acetic acid (170.4 g).

후처리

  1. temperaturewith heating at 84° C.-86° C. for 4 hours
  2. temperatureThe reaction mixture is cooled
  3. stirringThe mixture is stirred
  4. customthe aqueous layer is collected
  5. filtrationthe precipitated crystals are collected by filtration
  6. washwashed with water
  7. customdried with air at 60° C. for 15 hours

출처 및 근거

ORD 기록
ord-aad2945f10194c0d86862b7871db640d
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07262304B2

연결된 노트

불러오는 중…