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

Trifluoroacetic acid → HCID 89961656, 화합물

HRID 1521577
노트
인쇄 미리보기

반응식

HRID 1521577 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[CH:8]=[CH:9][C:10]3[NH:16][C:15](=S)[CH2:14][CH2:13][CH2:12][C:11]=3[CH:18]=2)[CH:2]=1.[F:19][C:20]([F:26])([F:25])[C:21]([NH:23][NH2:24])=O.C1(O)CCCCC1.FC(F)(F)C(O)=O>CS(C)=O>[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[CH:8]=[CH:9][C:10]3[N:16]4[C:21]([C:20]([F:26])([F:25])[F:19])=[N:23][N:24]=[C:15]4[CH2:14][CH2:13][CH2:12][C:11]=3[CH:18]=2)[CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6422Trifluoroacetic acidHCID 7966CyclohexanolHCID 229753TrifluoroacetohydrazideHCID 899616802H-1-Benzazepine-2-thione, 1,3,4,5-tetrahydro-7-(3-pyridinyl)-

생성물 1

HCID 89961656HCID 89961656, 화합물

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
120 °C

실험 절차

A flask containing the title compound from Example 2 Step E (9.0 mg, 0.04 mmol), 2,2,2-trifluoroacetohydrazide (3.2 mg, 0.04 mmol) and cyclohexanol (0.50 mL) was heated at 120° C. overnight. The reaction was then concentrated to give a residue that was diluted with dimethylsulfoxide, acidified with trifluoroacetic acid, and passed through a syringe filter before being purified by reverse phase HPLC (C18 column, 10 to 100% acetonitrile/water, both 0.1% v/v trifluoroacetic acid). Fractions containing product were combined, 1 M hydrochloric acid was added, and the solution concentrated to provide the title compound: LCMS m/z 330.99 [M+H]+; 1H NMR (500 MHz, CDCl3) δ 9.09 (br s, 1H), 8.76 (br s, 1H), 8.26 (d, J=Hz, 1H), 7.75-7.59 (m, 4H), 3.34 (br s, 1H), 2.90-2.85 (m, 1H), 2.52-2.40 (m, 3H), 2.27 (br s, 1H).

후처리

  1. concentrationThe reaction was then concentrated
  2. customto give a residue that
  3. custompassed through a syringe
  4. filtrationfilter
  5. custombefore being purified by reverse phase HPLC (C18 column, 10 to 100% acetonitrile/water
  6. additionFractions containing product
  7. addition1 M hydrochloric acid was added
  8. concentrationthe solution concentrated

출처 및 근거

ORD 기록
ord-47b94a4c01cb4abb9b14fd64f570a219
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09073929B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트