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

3-Thiophencarboxamide,N-methyl- → HCID 10244631, 화합물

HRID 1437141
노트
인쇄 미리보기

반응식

HRID 1437141 반응식
[CH3:1][NH:2][C:3]([C:5]1[CH:9]=[CH:8][S:7][CH:6]=1)=[O:4].O[CH2:11][NH:12][C:13](=[O:18])[C:14]([F:17])([F:16])[F:15]>S(=O)(=O)(O)O.C(OCC)(=O)C.C(=O)([O-])O.[Na+]>[CH3:1][NH:2][C:3]([C:5]1[CH:9]=[C:8]([CH2:11][NH:12][C:13](=[O:18])[C:14]([F:17])([F:16])[F:15])[S:7][CH:6]=1)=[O:4]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 8195533-Thiophencarboxamide,N-methyl-HCID 30849312,2,2-Trifluoro-N-(hydroxymethyl)acetamide

생성물 1

HCID 10244631HCID 10244631, 화합물

시약·촉매·용매 3

HCID 1118Sulfuric Acid용매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매2회

반응 조건

온도
20 °C

실험 절차

To suspension of N-methyl-3-thiophenecarboxamide (1.12 g) (prepared according to J. Org. Chem. (1976), 41(23), 3668-74) in concentrated aqueous sulphuric acid (25 ml) at 0-5° C. was added N-(hydroxymethyl)trifluoroacetamide (1.134 g). The suspension was allowed to warm to 20° C. and stirred for 2 h. The mixture was poured onto ice (150 g) and diluted with ethyl acetate (200 ml). The biphase mixture was diluted with saturated sodium hydrogen carbonate (200 ml) and treated with sodium hydrogen carbonate (21 g). The phases were separated and the organic phase washed with saturated sodium hydrogen carbonate (150 ml×2). The combined aqueous phases were extracted with ethyl acetate (100 ml). The combined organic extracts were concentrated in vacuo. The residue was pre-absorbed onto silica and purified by biotage (90 g) eluting with 1:1 to 0:1 cyclohexane:ethyl acetate to give the title compound as a white solid (0.7129).

후처리

  1. additionThe mixture was poured onto ice (150 g)
  2. customThe phases were separated
  3. washthe organic phase washed with saturated sodium hydrogen carbonate (150 ml×2)
  4. extractionThe combined aqueous phases were extracted with ethyl acetate (100 ml)
  5. concentrationThe combined organic extracts were concentrated in vacuo
  6. customThe residue was pre-absorbed onto silica
  7. custompurified by biotage (90 g)
  8. washeluting with 1:1 to 0:1 cyclohexane

출처 및 근거

ORD 기록
ord-be5173694d8d4c139d62c84e87399bc1
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07622464B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트