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

Sodium Iodide → HCID 22995793, 화합물

HRID 1167173
노트
인쇄 미리보기

반응식

HRID 1167173 반응식
C(N(C(C)C)CC)(C)C.[CH2:10]1[CH:15]2[CH2:16][NH:17][CH2:18][CH2:19][N:14]2[CH2:13][C:12](=[O:20])[O:11]1.FC(F)(F)C(O)=O.[Cl:28][C:29]1[CH:30]=[C:31]([NH:36][C:37]2[C:46]3[C:41](=[CH:42][C:43]([O:52][CH2:53][CH2:54]Br)=[C:44]([O:47][CH2:48][CH:49]4[CH2:51][CH2:50]4)[CH:45]=3)[N:40]=[CH:39][N:38]=2)[CH:32]=[CH:33][C:34]=1[F:35].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>C(#N)C>[Cl:28][C:29]1[CH:30]=[C:31]([NH:36][C:37]2[C:46]3[C:41](=[CH:42][C:43]([O:52][CH2:53][CH2:54][N:17]4[CH2:18][CH2:19][N:14]5[CH:15]([CH2:10][O:11][C:12](=[O:20])[CH2:13]5)[CH2:16]4)=[C:44]([O:47][CH2:48][CH:49]4[CH2:51][CH2:50]4)[CH:45]=3)[N:40]=[CH:39][N:38]=2)[CH:32]=[CH:33][C:34]=1[F:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 6

HCID 5238Sodium IodideHCID 6422Trifluoroacetic acid2회HCID 11430Potassium Carbonate2회HCID 81531DiisopropylethylamineHCID 18762784HCID 18762784, 화합물HCID 22989513Hexahydropyrazino[2,1-c][1,4]oxazin-3(4H)-one2회

생성물 1

HCID 22995793
HCID 22995793, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

0.25 ml of diisopropylethylamine and 260 mg of perhydro-pyrazino[2,1-c][1,4]oxazin-3-one x 2 trifluoroacetic acid are added to 150 mg of 4-[(3-chloro-4-fluorophenyl)amino]-6-cyclopropylmethoxy-7-(2-bromoethoxy)-quinazoline in 15 ml of acetonitrile. The reaction mixture is stirred for one hour at ambient temperature and then refluxed for two hours. Then 70 mg of potassium carbonate and 75 mg of sodium iodide are added. The reaction mixture is refluxed for about another 14 hours, during which time a total of another 175 mg of perhydro-pyrazino[2,1-c][1,4]oxazin-3-one x 2 trifluoroacetic acid and 300 mg of potassium carbonate are added successively until the reaction is complete. For working up the inorganic salts are filtered off and the filtrate is evaporated down in vacuo. The flask residue is chromatographed over a silica gel column with methylene chloride/methanol (95:5) as eluant. The desired product is obtained as a light brown resin. Yield: 27 mg (16% of theory),

후처리

  1. temperaturerefluxed for two hours
  2. additionare added successively until the reaction
  3. filtrationare filtered off
  4. customthe filtrate is evaporated down in vacuo
  5. customThe flask residue is chromatographed over a silica gel column with methylene chloride/methanol (95:5) as eluant

출처 및 근거

ORD 기록
ord-c521884d0d0244d5a01a162e44e25c4b
출처 데이터셋
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06617329B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트