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

Triethylamine → 2-(4-Bromo-2,6-difluorophenyl)-2-(4-ethyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)acetamide

HRID 1525934
노트
인쇄 미리보기

반응식

HRID 1525934 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([CH:9](O)[C:10]([NH2:12])=[O:11])=[C:4]([F:14])[CH:3]=1.C(N(CC)CC)C.CS(Cl)(=O)=O.S([O-])(=O)(=O)C.Cl.[CH2:33]([N:35]1[CH2:40][C:39]2([CH2:45][CH2:44][NH:43][CH2:42][CH2:41]2)[O:38][CH2:37][C:36]1=[O:46])[CH3:34]>C(#N)C>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[C:5]([CH:9]([N:43]2[CH2:44][CH2:45][C:39]3([O:38][CH2:37][C:36](=[O:46])[N:35]([CH2:33][CH3:34])[CH2:40]3)[CH2:41][CH2:42]2)[C:10]([NH2:12])=[O:11])=[C:4]([F:14])[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 8471Triethylamine2회HCID 31297Methanesulfonyl chlorideHCID 85257MethanesulfonateHCID 712710764-Ethyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochlorideHCID 712710952-(4-Bromo-2,6-difluorophenyl)-2-hydroxyacetamide

생성물 1

HCID 71270829
2-(4-Bromo-2,6-difluorophenyl)-2-(4-ethyl-3-oxo-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)acetamide
수율 121.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
40 °C

실험 절차

To a solution of 2-(4-bromo-2,6-difluorophenyl)-2-hydroxyacetamide (0.86 g, 3.2 mmol) and triethylamine (1.4 mL, 9.7 mmol) in anhydrous acetonitrile (5 mL) was added neat methanesulfonyl chloride (0.33 mL, 4.2 mmol). The reaction mixture was stirred vigorously at 40° C. for 3 h, at which point the reaction had progressed to completion. To this mesylate intermediate mixture was added more triethylamine (1.4 mL, 9.7 mmol) followed by 4-ethyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride (0.11 g, 0.48 mmol). The reaction mixture was heated at 90° C. for 3 h until the starting material was consumed. The reaction was diluted with water and was extracted with ether (3×35 mL). The combined ether phases were dried over sodium sulfate, filtered, and evaporated under reduced pressure. Purification of the residue by flash chromatography (65-100% of 10% methanol in dichloromethane:dichloromethane) afforded the title product (261 mg, 18% yield). MS(ES)+ m/e 446 [M+H]+; 1H NMR (400 MHz, CD2Cl2) δ ppm 1.12 (t, J=7.20 Hz, 3 H) 1.64-1.71 (m, 1 H) 1.73 (dd, J=4.17, 2.65 Hz, 1 H) 1.90-1.99 (m, 2 H) 2.19-2.27 (m, 1 H) 2.54-2.66 (m, 1 H) 2.67-2.73 (m, 1 H) 2.75-2.81 (m, 1 H) 3.15 (s, 2 H) 3.41 (q, J=6.91 Hz, 2 H) 3.98 (s, 2 H) 4.69 (s, 1 H) 5.68 (br. s., 1 H) 7.15-7.25 (m, 2 H) 7.36 (br. s., 1 H).

후처리

  1. temperatureThe reaction mixture was heated at 90° C. for 3 h until the starting material
  2. customwas consumed
  3. additionThe reaction was diluted with water
  4. extractionwas extracted with ether (3×35 mL)
  5. dry with materialThe combined ether phases were dried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customPurification of the residue by flash chromatography (65-100% of 10% methanol in dichloromethane:dichloromethane)

출처 및 근거

ORD 기록
ord-0817fa3046784d9a99f99c62ea48fc7d
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09084794B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트