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

2-Aminothiazole → HCID 86649623, 화합물

HRID 1897935
노트
인쇄 미리보기

반응식

HRID 1897935 반응식
Cl[C:2]1[N:7]=[C:6]([CH2:8][C:9]2([OH:22])[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:5]=[CH:4][CH:3]=1.[NH2:23][C:24]1[S:25][CH:26]=[CH:27][N:28]=1.CC1(C)C2C=CC=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=2OC2C1=CC=CC=2P(C1C=CC=CC=1)C1C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+].C(=O)([O-])[O-].[Cs+].[Cs+]>C(Cl)(Cl)Cl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].C1(C)C=CC=CC=1>[OH:22][C:9]1([CH2:8][C:6]2[CH:5]=[CH:4][CH:3]=[C:2]([NH:23][C:24]3[S:25][CH:26]=[CH:27][N:28]=3)[N:7]=2)[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 21552-AminothiazoleHCID 10340Sodium CarbonateHCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)2회HCID 57366393HCID 57366393, 화합물

생성물 1

HCID 86649623HCID 86649623, 화합물

시약·촉매·용매

3
HCID 6505921(1E,4E)-1,5-diphenylpenta-1,4-dien-3-one; palladium촉매2회HCID 1140Toluene용매HCID 6212Chloroform용매

반응 조건

온도
120 °C

실험 절차

A mixture of 50.3 mg of tert-butyl 4((6-chloropyridin-2-yl)methyl)-4-hydroxypiperidine-1-carboxylate, 19.3 mg of 2-aminothiazole, 9.0 mg of 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene, 4.8 mg of bis(dibenzylideneacetone)palladium(0), 25.2 mg of sodium carbonate and 0.77 ml of toluene was stirred at 100° C. overnight and 120° C. overnight. 156.6 mg of cesium carbonate, 94.4 mg of 9,9-dimethyl-4,5-bis(diphenylphosphino)xanthene and 47.1 mg of bis(dibenzylideneacetone)palladium(0) were added to the reaction mixture, followed by stirring the reaction mixture at 130° C. overnight. The reaction mixture was cooled to room temperature, and diluted with chloroform. An insoluble matter was filtered off using Celite, and the filtrate was concentrated in vacuo. The resulting residue was purified by a preparative thin-layer chromatography (Kieselgel™ 60F254, Art5744 (Merck), chloroform/methanol=10/1) to give the title compound as a brown oil.

후처리

  1. stirringby stirring the reaction mixture at 130° C. overnight
  2. temperatureThe reaction mixture was cooled to room temperature
  3. filtrationAn insoluble matter was filtered off
  4. concentrationthe filtrate was concentrated in vacuo
  5. customThe resulting residue was purified by a preparative thin-layer chromatography (Kieselgel™ 60F254, Art5744 (Merck), chloroform/methanol=10/1)

출처 및 근거

ORD 기록
ord-114a40bf5c464761b5cae7ac4fc4ed1a
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08519136B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트