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

Formic Acid → HCID 12246022, 화합물

HRID 268529
노트
인쇄 미리보기

반응식

HRID 268529 반응식
[C:1](OC(=O)C)(=O)C.C(O)=O.[NH2:11][N:12]1[C:21]([OH:28])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:20]2[C:15](=[CH:16][CH:17]=[C:18]([Cl:29])[CH:19]=2)[N:14]=[CH:13]1>C(O)(=O)C>[Cl:29][C:18]1[CH:17]=[CH:16][C:15]([N:14]2[CH:1]=[N:11][N:12]=[CH:13]2)=[C:20]([CH:19]=1)[C:21]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 284Formic AcidHCID 7918Acetic AnhydrideHCID 1196793-Amino-6-chloro-3,4-dihydro-4-phenylquinazolin-4-ol

생성물 1

HCID 12246022HCID 12246022, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A stirred solution of acetic anhydride (25.3 ml) and 97% formic acid (10.6 ml) is kep at ambient temperature (25°) for 30 minutes, cooled in an ice bath and treated with 3-amino-6-chloro-3,4-dihydro-4-hydroxy-4-phenylquinazoline (12.24 g, 0.0447 mole). The solution is kept at ambient temperature for 18 hours, diluted with acetic acid (25 ml), warmed to the reflux temperature during 1 hour and refluxed for 1.5 hours. The solution is concentrated in vacuo, and the residue is mixed with cold water, made alkaline with sodium hydroxide and extracted with chloroform. The extract is washed with brine, dried over anhydrous sodium sulfate and concentrated. The residue is crystallized from ethylacetate to give 7.76 g of 5-chloro-2-(4H-1,2,4-triazol-4-yl)-benzophenone of melting point 184°-186° C., 0.971 g of melting point 182.5°-184° C., and 0.144 of melting point 181°-182° C.

후처리

  1. customis kep at ambient temperature
  2. custom(25°)
  3. customfor 30 minutes
  4. temperaturecooled in an ice bath
  5. temperaturewarmed to the reflux temperature during 1 hour
  6. temperaturerefluxed for 1.5 hours
  7. concentrationThe solution is concentrated in vacuo
  8. additionthe residue is mixed with cold water
  9. extractionextracted with chloroform
  10. washThe extract is washed with brine
  11. dry with materialdried over anhydrous sodium sulfate
  12. concentrationconcentrated
  13. customThe residue is crystallized from ethylacetate

출처 및 근거

ORD 기록
ord-f34a287504f4477fa97fd29e2df15af9
출처 데이터셋
uspto-grants-1976_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03947466

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트