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Hydrochloric Acid → HCID 178482338、化合物

HRID 340843
ノート
印刷プレビュー

反応式

HRID 340843 の反応式
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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

13

反応物 9

HCID 313Hydrochloric AcidHCID 6329Methylamine2 回HCID 63651,1-DichloroethaneHCID 24819Phosphorus pentachloride2 回HCID 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、化合物

生成物 1

HCID 178482338HCID 178482338、化合物収率 89%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
-78 °C

実験手順

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)+.

後処理

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

出典と根拠

ORDレコード
ord-ff7943c480c14de9b3eb54c47dab7dc2
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895545B2

反応ノート

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