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Triisopropyl phosphate → 2-[2,6-Dichloro-4-(ethylthio)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepine bis(trifluoroacetate)

HRID 75232
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HRID 75232 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[N:8]1[C:13]2[NH:14][C:15]3[CH:25]=[N:24][CH:23]=[CH:22][C:16]=3/[C:17](=[N:20]/O)/[C:18](=O)[C:12]=2[CH:11]=[CH:10][CH:9]=1.[Cl:26][C:27]1[CH:34]=[C:33]([S:35][CH2:36][CH3:37])[CH:32]=[C:31]([Cl:38])[C:28]=1[CH:29]=O.C([O-])(=O)C.[NH4+:43].P(OC(C)C)(OC(C)C)(OC(C)C)=O>C(O)(=O)C.C(#N)C>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[Cl:26][C:27]1[CH:34]=[C:33]([S:35][CH2:36][CH3:37])[CH:32]=[C:31]([Cl:38])[C:28]=1[C:29]1[NH:20][C:17]2[C:16]3[CH:22]=[CH:23][N:24]=[CH:25][C:15]=3[NH:14][C:13]3[N:8]=[CH:9][CH:10]=[CH:11][C:12]=3[C:18]=2[N:43]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 68188Triisopropyl phosphateHCID 517165Ammonium AcetateHCID 866132762,6-Dichloro-4-(ethylthio)benzaldehydeHCID 178525666HCID 178525666, 화합물

생성물 1

HCID 866132772-[2,6-Dichloro-4-(ethylthio)phenyl]-3,8-dihydroimidazo[4,5-d]dipyrido[2,3-b:4',3'-f]azepine bis(trifluoroacetate)

시약·촉매·용매 2

HCID 176
Acetic Acid
용매
HCID 6342Acetonitrile용매

반응 조건

온도
130 °C

실험 절차

A solution of (6Z)-5H-dipyrido[2,3-b:4′,3′-f]azepine-5,6(11H)-dione 6-oxime trifluoroacetate (200 mg, 0.4 mmol), 2,6-dichloro-4-(ethylthio)benzaldehyde (200 mg, 0.85 mmol) and ammonium acetate (0.60 g, 8.0 mmol) were stirred in acetic acid (3 mL) and heated in a microwave for 5 minutes at 130° C. Evaporation gave the crude product which was dissolved in acetonitrile (1.0 mL) and triisopropyl phosphate (100 μL, 0.4 mmol) and heated in a microwave for 5 minutes at 180° C. Purification by preparative LCMS gave the desired product LC/MS: 440 (M+H)+.

후처리

  1. customEvaporation
  2. customgave the crude product which
  3. customPurification by preparative LCMS

출처 및 근거

ORD 기록
ord-7a4d5407d9334c629fad306666b78b57
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08835423B2

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