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Acetic Acid → (S)-2-tert-butoxy-2-(7-(4-chlorophenyl)-5-methyl-2-(1-methyl-3-(4-methylpiperazin-1-yl)-1H-indazol-5-yl)benzo[d]thiazol-6-yl)acetic acid

HRID 879483
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HRID 879483 반응식
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([CH3:11])[N:6]=[C:5]2[N:12]1[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]1.C(Cl)Cl.CC(O)=O.CC([O-])=O.[K+].Br[C:32]1[S:33][C:34]2[C:40]([C:41]3[CH:46]=[CH:45][C:44]([Cl:47])=[CH:43][CH:42]=3)=[C:39]([C@H:48]([O:54][C:55]([CH3:58])([CH3:57])[CH3:56])[C:49]([O:51]CC)=[O:50])[C:38]([CH3:59])=[CH:37][C:35]=2[N:36]=1.C([O-])([O-])=O.[K+].[K+].[OH-].[Na+]>C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCO.O1CCOCC1>[C:55]([O:54][C@@H:48]([C:39]1[C:38]([CH3:59])=[CH:37][C:35]2[N:36]=[C:32]([C:2]3[CH:3]=[C:4]4[C:8](=[CH:9][CH:10]=3)[N:7]([CH3:11])[N:6]=[C:5]4[N:12]3[CH2:17][CH2:16][N:15]([CH3:18])[CH2:14][CH2:13]3)[S:33][C:34]=2[C:40]=1[C:41]1[CH:42]=[CH:43][C:44]([Cl:47])=[CH:45][CH:46]=1)[C:49]([OH:51])=[O:50])([CH3:58])([CH3:56])[CH3:57]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 7

HCID 176Acetic AcidHCID 6344DichloromethaneHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 517044Potassium AcetateHCID 858434475-bromo-1-methyl-3-(4-methylpiperazin-1-yl)-1H-indazoleHCID 86700141
(S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate

생성물 1

HCID 72196116(S)-2-tert-butoxy-2-(7-(4-chlorophenyl)-5-methyl-2-(1-methyl-3-(4-methylpiperazin-1-yl)-1H-indazol-5-yl)benzo[d]thiazol-6-yl)acetic acid

시약·촉매·용매 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매HCID 178418397HCID 178418397, 화합물촉매HCID 702Ethanol용매HCID 312751,4-Dioxane용매

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온도
100 °C

실험 절차

A vial was charged with 5-bromo-1-methyl-3-(4-methylpiperazin-1-yl)-1H-indazole (64.0 mg, 0.208 mmol), bis-pinacolatodiboron (58 mg, 0.23 mmol), PdCl2(dppf).DCM (17 mg, 21 μmol), glacial AcOH (13 μL, 0.23 mmol), KOAc (67 mg, 0.69 mmol), and dioxane (1.6 mL). The reaction was heated to 100° C. for 2 h. To this reaction was added (S)-ethyl 2-(2-bromo-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (103 mg, 0.208 mmol), KHCO3 (23 mg, 0.23 mmol), 2 M aq K2CO3 (400 μL), and Pd(PPh3)4 (24 mg, 21 μmol). The reaction was heated for another 1 h at 100° C. Finally, EtOH (absolute, 800 μL) and 10 M aq NaOH (500 μL) were added. The reaction was heated to 100° C. for another 1 h. The reaction was cooled to 23° C., and filtered (0.45 micron teflon syringe filter). The filtrate was purified by reverse phase HPLC, eluting by 5-100% acetonitrile in H2O with 0.1% TFA to give the desired product. LCMS-ESI+: calc'd for C33H36ClN5O3S: 618.2, 620.2 (M+H+); Found: 618.4, 620.2 (M+H+). 1H NMR (400 MHz, CD3OD): δ 8.43 (s, 1H), 8.05 (d, J=8.9 Hz, 1H), 7.80 (s, 1H), 7.68 (d, J=9.1 Hz, 1H), 7.62-7.47 (m, 4H), 5.24 (s, 1H), 4.31-4.01 (m, 2H), 3.94 (s, 3H), 3.74-3.54 (m, 2H), 3.54-3.35 (m, 2H), 3.32-3.16 (m, 2H), 3.00 (s, 3H), 2.61 (s, 3H), 0.97 (s, 9H).

후처리

  1. temperatureThe reaction was heated for another 1 h at 100° C
  2. temperatureThe reaction was heated to 100° C. for another 1 h
  3. temperatureThe reaction was cooled to 23° C.
  4. filtrationfiltered
  5. filtration(0.45 micron teflon syringe filter)
  6. customThe filtrate was purified by reverse phase HPLC
  7. washeluting by 5-100% acetonitrile in H2O with 0.1% TFA

출처 및 근거

ORD 기록
ord-9c6b9e6e772244128656462af94f3bc9
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08987250B2

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