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Water → HCID 21191969, 화합물

HRID 1069816
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HRID 1069816 반응식
[OH:1][C:2]1[C:11]([C:12]([OH:14])=[O:13])=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:15]([OH:17])=[O:16])[CH:8]=2)[CH:3]=1.[Br:18]Br.O>C(Cl)(Cl)Cl.CS(C)=O>[Br:18][C:3]1[C:4]2[C:9](=[CH:8][C:7]([C:15]([OH:17])=[O:16])=[CH:6][CH:5]=2)[CH:10]=[C:11]([C:12]([OH:14])=[O:13])[C:2]=1[OH:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 962WaterHCID 24408BromineHCID 98160552-Hydroxynaphthalen-3,6-dicarboxylic acid

생성물 1

HCID 21191969HCID 21191969, 화합물수율 97%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 6212Chloroform용매2회

실험 절차

2-Hydroxy-3,6-di-hydroxycarbonylnaphthalene (11.8 g) was dissolved in chloroform (300 g) and dimethyl sulfoxide (100 g), followed by ice-cooling. Then, a solution of bromine (8.0 g) and chloroform (50 g) was added dropwise at not more than 5° C. over 2 hours. After continuously stirring for 1 hour, this solution was poured into water (1500 g) dropwise. The deposit was filtered and then washed with water and dispersed in a small amount of methanol. The dispersion was concentrated under reduced pressure at room temperature and then dried under vacuum to obtain 15.1 g of 1-bromo-2-hydroxy-3,6-di-hydroxycarbonylnaphthalene as a whitish brown crystal (DSC analysis value: 145.2° C.).

후처리

  1. temperaturecooling
  2. filtrationThe deposit was filtered
  3. washwashed with water
  4. additiondispersed in a small amount of methanol
  5. concentrationThe dispersion was concentrated under reduced pressure at room temperature
  6. customdried under vacuum

출처 및 근거

ORD 기록
ord-5b2c30495ec24c74a62f090f2275b322
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06252104B1

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