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Hydrochloric Acid → HCID 178482338, 화합물

HRID 340843
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HRID 340843 반응식
P(Cl)(Cl)(Cl)(Cl)[Cl:2].NC.[CH3:9][N:10]([CH2:15][C:16]1[O:17][C:18]2[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=2[C:20]=1[CH3:21])[C:11](=[O:14])[CH:12]=[CH2:13].CCN(C(C)C)C(C)C.CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C.Cl.Br[C:59]1[CH:68]=[N:67][C:66]2[NH:65]/[C:64](=[N:69]/[CH3:70])/[C:63]([CH3:72])([CH3:71])[O:62][C:61]=2[CH:60]=1.ClC(Cl)C.BrC1C=NC2NC(=O)C(C)(C)OC=2C=1>C(Cl)Cl.CC([O-])=O.CC([O-])=O.[Pd+2].CN(C=O)C>[ClH:2].[CH3:71][C:63]1([CH3:72])[O:62][C:61]2[CH:60]=[C:59](/[CH:13]=[CH:12]/[C:11]([N:10]([CH3:9])[CH2:15][C:16]3[O:17][C:18]4[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=4[C:20]=3[CH3:21])=[O:14])[CH:68]=[N:67][C:66]=2[NH:65]/[C:64]/1=[N:69]/[CH3:70]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

13

반응물 9

HCID 313Hydrochloric AcidHCID 6329Methylamine2회HCID 63651,1-DichloroethaneHCID 24819Phosphorus pentachloride2회HCID 80271Tri-o-tolylphosphineHCID 81531DiisopropylethylamineHCID 577420407-bromo-2,2-dimethyl-2H,3H,4H-pyrido(3,2-b)(1,4)oxazin-3-one
HCID 57742103N-methyl-N-(3-methylbenzofuran-2-ylmethyl)acrylamide
HCID 178482337HCID 178482337, 화합물

생성물 1

HCID 178482338HCID 178482338, 화합물수율 89%

시약·촉매·용매 3

HCID 167845palladium(II) acetate촉매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

반응 조건

온도
-78 °C

실험 절차

Reagents and conditions: a) PCl5, μwave then NH2Me, b) N-methyl-N-((3-methylbenzofuran-2-yl)methyl)acrylamide, DIPEA, Pd(OAc)2, P(o-Tol)3, DMF, then HCl. a) (E)-N-(7-bromo-2,2-dimethyl-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-ylidene)methanamine: A dichloroethane (5 mL) solution of 7-bromo-2,2-dimethyl-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-one (520 mg, 2 mmol) and phosphorus pentachloride (840 mg, 4 mmol) was irradiated in a microwave oven for 10 min at. 160° C. The solution was cooled to −78° C. and methylamine (2M in THF) was added it slowly until it became permanently basic. The mixture was diluted with CH2Cl2, washed with dilute solution of NaOH, dried, and evaporated. Crystallization from CH2Cl2/hexane afforded 480 mg (89%) of the title compound. 1H NMR (300 MHz, CDCl3, δ) 8.07 (d, J=2.1 Hz, 1H), 7.21 (d, J=2.1 Hz, 1H), 4.9 (s, br, 1H), 3.06 (d, J=4.5 Hz, 3H), 1.46 (s, 6H). MS (ESI) m/e 270 (M+H)+. b) (E)-3-((E)-2,2-dimethyl-3-(methylimino)-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-7-yl)-N-methyl-N-((3-methylbenzofuran-2-yl)methyl)acrylamide: A DMF (3 mL) solution of (E)-N-(7-bromo-2,2-dimethyl-2H-pyrido[3,2-b][1,4]oxazin-3(4H)-ylidene)methanamine (271 mg, 1 mmol), N-methyl-N-((3-methylbenzofuran-2-yl)methyl)acrylamide (345 mg, 1.5 mmol) and diisopropylethylamine (0.52 mL, 3 mmol) was purged with Argon for 10 min. Pd(OAc)2 (24 mg, 0.1 mmol) and P(o-tol)3 (61 mg, 0.2 mmol) was added and then the Argon purge was repeated. The mixture was irradiated in a microwave oven for 10 min at 160° C. under Argon. Upon cooling, the mixture was diluted with water and extracted with EtOAc. The crude product was purified by chromatography (silica, 0-4% MeOH in CH2Cl2). The free base was turned into the HCl salt by addition of HCl (1 ml, 1M m Et2O) to its CH2Cl2 solution and evaporation to afford 230 mg (55%) of the title compound, as a mixture of amide rotamers. 1H NMR (300 MHz, CDCl3, δ, free base) 8.20 (s, 1H), 7.69 and 7.85 (2s, 1H), 7.5-6.7 (m, 6H), 5.14 (s, br, 1H), 4.83 and 4.71 (2s, 2H), 3.21 and 3.10 (2s, 3H), 3.09 (d, J=4.8 Hz, 3H), 2.31 (s, 3H), 1.49 (s, 6H). MS (ESI) m/e 419 (M+H)+.

후처리

  1. custom160° C
  2. washwashed with dilute solution of NaOH
  3. customdried
  4. customevaporated
  5. customCrystallization from CH2Cl2/hexane

출처 및 근거

ORD 기록
ord-ff7943c480c14de9b3eb54c47dab7dc2
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895545B2

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