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Morpholine → HCID 57635415、化合物

HRID 1971101
ノート
印刷プレビュー

反応式

HRID 1971101 の反応式
BrC1N2CCN(C)CC2=[C:4]([C:12]([NH:14][C@@H:15](C(C)(C)C)[C:16](NC)=[O:17])=O)N=1.[CH3:24][C:25]([CH3:53])([CH3:52])[C@H:26]([NH:31][C:32]([C:34]1[N:35]=[C:36]([C:44]#[C:45][C:46]2C=CC=CC=2)[N:37]2[CH2:42][CH2:41][N:40]([CH3:43])[CH2:39][C:38]=12)=[O:33])[C:27]([NH:29][CH3:30])=[O:28].ClC/C=C/B(O)O.C([O-])([O-])=O.[K+].[K+].N1CCOCC1>O1CCOCC1.CCOC(C)=O.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.O>[CH3:24][C:25]([CH3:53])([CH3:52])[C@H:26]([NH:31][C:32]([C:34]1[N:35]=[C:36](/[CH:44]=[CH:45]/[CH2:46][N:14]2[CH2:12][CH2:4][O:17][CH2:16][CH2:15]2)[N:37]2[CH2:42][CH2:41][N:40]([CH3:43])[CH2:39][C:38]=12)=[O:33])[C:27]([NH:29][CH3:30])=[O:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 5

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 6080110B-[(1E)-3-Chloro-1-propen-1-yl]boronic acidHCID 57635127HCID 57635127、化合物HCID 57635398HCID 57635398、化合物

生成物 1

HCID 57635415HCID 57635415、化合物収率 34%

試薬・触媒・溶媒

4
HCID 178418397HCID 178418397、化合物触媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒HCID 312751,4-Dioxane溶媒

実験手順

(S)-3-bromo-N-(3,3-dimethyl-1-(methylamino)-1-oxobutan-2-yl)-7-methyl-5,6,7,8-tetrahydroimidazo[1,5-a]pyrazine-1-carboxamide (Compound 203; 0.12 g, 0.31 mmol) was dissolved in dioxane (4 mL) and (E)-3-chloroprop-1-enylboronic acid (0.037 g, 0.31 mmol) was added, followed by K2CO3 (0.11 g, 0.82 mmol), morpholine (0.054 g, 0.66 mmol) and water (0.80 mL). The resulting mixture was degassed with nitrogen and Pd(PPh3)4 (0.019 g, 0.017 mmol) was added. The mixture was subjected to microwave irradiation at 160° C. for 20 min. The mixture was diluted with EtOAc, and filtered through celite. The organic layer was concentrated, washed with water, dried over anhydrous Na2SO4, filtered and concentrated again. The residue was purified by prep LC/MS using 5-95% gradient acetonitrile/water with 0.1% formic acid to provide Compound 286 (0.035 g, 34%) as a yellow solid. 1H-NMR (400 MHz, CDCl3) δ: 1.07 (s, 9H), 2.52 (s, 3H), 2.81 (d, 3H), 2.89 (t, 2H), 2.97 (m, 3H), 3.28 (s, 1H), 3.58 (d, 1H), 3.99 (m, 8H), 4.35 (d, 1H), 6.11 (m, 1H), 6.68 (m, 2H), 7.71 (m, 1H); LCMS (+ESI) m/z 433.3 [M+H]+.

後処理

  1. additionwas added
  2. customirradiation at 160° C. for 20 min
  3. filtrationfiltered through celite
  4. concentrationThe organic layer was concentrated
  5. washwashed with water
  6. dry with materialdried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated again
  9. customThe residue was purified by prep LC/MS

出典と根拠

ORDレコード
ord-b7796c6f95f24b018e7c91ab276c954a
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08431565B2

反応ノート

読み込み中…

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