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Sulfuric Acid → HCID 19423378, 화합물

HRID 1464180
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HRID 1464180 반응식
[OH:1][C:2]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][C:15]2[CH:20]=[CH:19][C:18]([S:21]([Cl:24])(=[O:23])=[O:22])=[CH:17][CH:16]=2)=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].S(=O)(=O)(O)O.[Cl-].[Na+].[C:32](OC(=O)C)(=[O:34])[CH3:33]>C1(C)C=CC=CC=1>[C:32]([O:1][C:2]1[CH:12]=[CH:11][C:10]([C:13]#[C:14][C:15]2[CH:20]=[CH:19][C:18]([S:21]([Cl:24])(=[O:23])=[O:22])=[CH:17][CH:16]=2)=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5])(=[O:34])[CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 5234Sodium ChlorideHCID 7918Acetic AnhydrideHCID 19423376Ethyl 2-hydroxy-5-[(4-chlorosulfonylphenyl]ethynyl]benzoate

생성물 1

HCID 19423378HCID 19423378, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Ethyl 2-hydroxy-5-[(4-chlorosulfonylphenyl]ethynyl]benzoate (16 g, 44 mmol) was dissolved in acetic anhydride (40 ml) at 120° C. Sulfuric acid (about 0.4 ml) was added dropwise. After 5 min the solution was diluted with toluene (about 100 ml) and added to saturated sodium chloride solution with vigorous stirring. The phases were separated, the toluene solution dried and evaporated. More toluene was added and the evaporation repeated. The oily product crystallized. The product was sufficiently pure for the next step. Yield 17.0 g (95%).

후처리

  1. customThe phases were separated
  2. dry with materialthe toluene solution dried
  3. customevaporated
  4. additionMore toluene was added
  5. customthe evaporation
  6. customThe oily product crystallized

출처 및 근거

ORD 기록
ord-3421f86c48ae450daf7dddbaf4e2615d
출처 데이터셋
uspto-grants-1994_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05302718

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