홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Acetic Acid → Dibenzo[b,f]thiepin-3-carboxaldehyde 5,5-dioxide

HRID 485099
노트
인쇄 미리보기

반응식

HRID 485099 반응식
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[CH:12]=[CH:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[S:8](=[O:18])(=[O:17])[C:7]=2[CH:19]=1)#N.N1C=CC=CC=1.C(O)(=[O:28])C.[PH2]([O-])=O.[Na+]>[Ni].O>[CH:5]1[C:6]2[CH:12]=[CH:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[S:8](=[O:18])(=[O:17])[C:7]=2[CH:19]=[C:3]([CH:1]=[O:28])[CH:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 1049PyridineHCID 13151874HCID 13151874, 화합물HCID 178527019HCID 178527019, 화합물

생성물 1

HCID 13520245Dibenzo[b,f]thiepin-3-carboxaldehyde 5,5-dioxide

시약·촉매·용매 2

HCID 935Nickel촉매
HCID 962
Water
용매

반응 조건

온도
25 °C

실험 절차

Mix 267 mg (1 mmole) of 3-cyano-dibenzo[b,f]thiepin-5,5-dioxide, 10 ml pyridine, 5 ml acetic acid, and 5 ml water. Add 0.5 g sodium hypophosphite and approximately 0.1 g Raney nickel. Stir at 25° C. for 24 hours and then at 45°-50° C. for 2 hours. Filter the reaction mixture to remove the catalyst and wash any product from the catalyst using 10 ml ethyl acetate. Add 10 ml 6N hydrochloric acid and separate the organic layer containing the product. Evaporate the organic layer to obtain a solid residue comprising the title product, m.p., 175°-177° C. Swishing with methanol and drying the residue gives product melting at 177°-178° C.

후처리

  1. waitat 45°-50° C. for 2 hours
  2. filtrationFilter the reaction mixture
  3. customto remove the catalyst
  4. washwash any product from the catalyst
  5. additionAdd 10 ml 6N hydrochloric acid
  6. customseparate the organic layer
  7. additioncontaining the product
  8. customEvaporate the organic layer
  9. customto obtain a solid residue

출처 및 근거

ORD 기록
ord-f25086cc72244b918ad76c1626d96615
출처 데이터셋
uspto-grants-1985_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04535171

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트