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Potassium Carbonate → 4-[(3-Chloro-2-fluoro-phenyl)amino]-6-(1,4-dioxa-spiro[4.5]decan-8-yl-oxy)-7-methoxy-quinazoline

HRID 1672122
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인쇄 미리보기

반응식

HRID 1672122 반응식
C(=O)([O-])[O-].[K+].[K+].CS([O:11][CH:12]1[CH2:21][CH2:20][C:15]2([O:19][CH2:18][CH2:17][O:16]2)[CH2:14][CH2:13]1)(=O)=O.[Cl:22][C:23]1[C:24]([F:43])=[C:25]([NH:29][C:30]2[C:39]3[C:34](=[CH:35][C:36]([O:41][CH3:42])=[C:37](O)[CH:38]=3)[N:33]=[CH:32][N:31]=2)[CH:26]=[CH:27][CH:28]=1>CN(C)C=O.O.C(OCC)(=O)C>[Cl:22][C:23]1[C:24]([F:43])=[C:25]([NH:29][C:30]2[C:39]3[C:34](=[CH:35][C:36]([O:41][CH3:42])=[C:37]([O:11][CH:12]4[CH2:21][CH2:20][C:15]5([O:19][CH2:18][CH2:17][O:16]5)[CH2:14][CH2:13]4)[CH:38]=3)[N:33]=[CH:32][N:31]=2)[CH:26]=[CH:27][CH:28]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11430Potassium Carbonate2회HCID 149667411,4-Dioxaspiro(4.5)decan-8-yl methanesulfonate2회HCID 574768684-((3-Chloro-2-fluorophenyl)amino)-7-methoxyquinazolin-6-ol

생성물 1

HCID 591581734-[(3-Chloro-2-fluoro-phenyl)amino]-6-(1,4-dioxa-spiro[4.5]decan-8-yl-oxy)-7-methoxy-quinazoline

시약·촉매·용매 3

HCID 962Water
용매
HCID 6228Dimethylformamide용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

At 50° C. 12.5 g potassium carbonate and 16 g 8-methanesulphonyloxy-1,4-dioxa-spiro[4,5]decane (cf for example Journal of Medicinal Chemistry (1992), 35(12), 2243-7) are added to 18.1 g 4-[(3-chloro-2-fluoro-phenyl)amino]-6-hydroxy-7-methoxy-quinazoline (cf for example Bioorganic & Medicinal Chemistry Letters (2006), 16(18), 4908-4912) in 125 ml dimethylformamide and the mixture is stirred for 18 hours at 80° C. Another 4.7 g potassium carbonate and 4.0 g of 8-methanesulphonyloxy-1,4-dioxa-spiro[4,5]decane are added and the mixture is stirred for another 7 hours at 80° C. The reaction mixture is cooled, diluted with water and ethyl acetate and the precipitate formed is suction filtered and dried.

후처리

  1. customAt 50° C
  2. stirringthe mixture is stirred for another 7 hours at 80° C
  3. temperatureThe reaction mixture is cooled
  4. customthe precipitate formed
  5. filtrationfiltered
  6. customdried

출처 및 근거

ORD 기록
ord-c921a31264244f518bb09e6c456b699d
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07998949B2

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