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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Benzyl mercaptan → HCID 11076271, 화합물

HRID 703039
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인쇄 미리보기

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HRID 703039 반응식
CC(C)([O-])C.[K+].[CH2:7]([SH:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.Cl[C:16]1[C:23]([Cl:24])=[CH:22][CH:21]=[CH:20][C:17]=1[CH:18]=[O:19]>CN(C)C=O>[Cl:24][C:23]1[C:16]([S:14][CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:17]([CH:20]=[CH:21][CH:22]=1)[CH:18]=[O:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7509Benzyl mercaptanHCID 357452,3-DichlorobenzaldehydeHCID 23665647Potassium tert-butoxide

생성물 1

HCID 11076271HCID 11076271, 화합물수율 76.5%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

반응 조건

온도
25 °C

실험 절차

To a suspension of 112.1 g of potassium-t-butoxide in 1000 mL of dimethylformamide under a nitrogen atmosphere, 124.3 g of benzylmercaptan was added dropwise while maintaining the reaction temperature at 20°-25° C. with an ice-water bath. After stirring at 25° C. for 1.5 hours, a solution of 175 g of 2,3-dichlorobenzaldehyde dissolved in 750 mL of N,N-dimethylformamide was added dropwise, while maintaining the reaction temperature at 25°-40° with a water bath. After stirring at 25° C. for 12 hours, the reaction mixture was poured onto excess ice water to yield a precipitate. The suspension was filtered, and the isolated solid was washed with water, suction-dried and finally dried in vacuo at 40° C. overnight to afford 201 g of the title compound as a light yellow solid; m.p. 65°-68° C.

후처리

  1. temperaturewhile maintaining the reaction temperature at 20°-25° C. with an ice-water bath
  2. additionwas added dropwise
  3. temperaturewhile maintaining the reaction temperature at 25°-40° with a water bath
  4. stirringAfter stirring at 25° C. for 12 hours
  5. customto yield a precipitate
  6. filtrationThe suspension was filtered
  7. washthe isolated solid was washed with water
  8. customsuction-dried
  9. customfinally dried in vacuo at 40° C. overnight

출처 및 근거

ORD 기록
ord-82552ca2f2064709ae1345a6b09bfb87
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04981506

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