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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Benzoyl chloride → HCID 15406406, 화합물

HRID 616629
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HRID 616629 반응식
[C:1]1([C:7]2[C:11]3[CH:12]=[CH:13][C:14]([O:16][CH3:17])=[CH:15][C:10]=3[S:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[Cl-].[Al+3].[Cl-].[Cl-]>ClCCCl>[C:18]([C:8]1[S:9][C:10]2[CH:15]=[C:14]([O:16][CH3:17])[CH:13]=[CH:12][C:11]=2[C:7]=1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) ChlorideHCID 15422638HCID 15422638, 화합물

생성물 1

HCID 15406406HCID 15406406, 화합물수율 52%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
0 °C

실험 절차

To 100 ml. of 1,2-dichloroethane were added 5.0 g. (0.021 mole) of 3-phenyl-6-methoxybenzothiophene and 2.81 g. (0.021 mole) of benzoyl chloride. The mixture was cooled to 0° C., and 2.93 g. (0.022 mole) of aluminum chloride were added. The mixture was stirred for one hour, and ice then was added. The resulting organic layer was separated, washed with water, and evaporated. To the residue were added 250 ml. of methanol and 10 ml. of 5N sodium hydroxide. The mixture was refluxed for 30 minutes, evaporated, and ether and water were added to the residue. The ether layer was separated, washed with 1N sodium hydroxide, 1N hydrochloric acid, and aqueous soidum chloride. The ether layer then was dried over magnesium sulfate, filtered, and evaporated. The residue was crystallized from methanol to obtain 3.77 g. (52 percent) of the title compound, m.p. 94°-95.5° C.

후처리

  1. additionice then was added
  2. customThe resulting organic layer was separated
  3. washwashed with water
  4. customevaporated
  5. additionTo the residue were added 250 ml
  6. temperatureThe mixture was refluxed for 30 minutes
  7. customevaporated
  8. additionether and water were added to the residue
  9. customThe ether layer was separated
  10. washwashed with 1N sodium hydroxide, 1N hydrochloric acid, and aqueous soidum chloride
  11. dry with materialThe ether layer then was dried over magnesium sulfate
  12. filtrationfiltered
  13. customevaporated
  14. customThe residue was crystallized from methanol
  15. customto obtain 3.77 g

출처 및 근거

ORD 기록
ord-8cad5b6157cb43d79cbec7d1ab51a421
출처 데이터셋
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04075227

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