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Diisopropylethylamine → HCID 178461980、化合物

HRID 75322
ノート
印刷プレビュー

反応式

HRID 75322 の反応式
Cl.C([O:9][C:10]1[CH:15]=[C:14]([C:16]2[CH:17]=[C:18]3[N:27]([CH3:28])[CH:26]=[CH:25][C:19]3=[N:20][C:21]=2[C@@H:22]([NH2:24])[CH3:23])[CH:13]=[CH:12][N:11]=1)C1C=CC=CC=1.Cl.N[C@H](C1N=C2C=CN(C)C2=CC=1C1C=CN=C(O)C=1)C.[NH2:50][C:51]1[N:56]=[C:55]([NH2:57])[C:54]([C:58]#[N:59])=[C:53](Cl)[N:52]=1.C(N(C(C)C)C(C)C)C>C(#N)C>[NH2:50][C:51]1[N:56]=[C:55]([NH2:57])[C:54]([C:58]#[N:59])=[C:53]([NH:24][C@H:22]([C:21]2[N:20]=[C:19]3[CH:25]=[CH:26][N:27]([CH3:28])[C:18]3=[CH:17][C:16]=2[C:14]2[CH:13]=[CH:12][N:11]=[C:10]([OH:9])[CH:15]=2)[CH3:23])[N:52]=1
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

6

反応物 4

HCID 81531DiisopropylethylamineHCID 867080212,4-Diamino-6-chloropyrimidine-5-carbonitrileHCID 86708023(S)-1-(6-(2-(benzyloxy)pyridin-4-yl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine hydrochlorideHCID 178461863HCID 178461863、化合物

生成物 1

HCID 178461980HCID 178461980、化合物収率 46.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
120 °C

実験手順

A mixture of (S)-1-(6-(2-(benzyloxy)pyridin-4-yl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-5-yl)ethanamine hydrochloride (155 mg, 0.393 mmol) and (S)-4-(5-(1-aminoethyl)-1-methyl-1H-pyrrolo[3,2-b]pyridin-6-yl)pyridin-2-ol hydrochloride (120 mg, 0.393 mmol) along with 2,4-diamino-6-chloropyrimidine-5-carbonitrile (100 mg, 0.590 mmol) and N-ethyl-N-isopropylpropan-2-amine (0.205 mL, 1.18 mmol) were combined in acetonitrile (6 mL). The reaction mixture was heated in a microwave reactor at 120° C. for 2 hours and then concentrated. The residue was dissolved in MeOH (10 mL). Pd/C (10%, 700 mg) was added and the reaction mixture was maintained under an atmosphere of hydrogen for 30 minutes. The mixture was filtered through Celite and concentrated. The residue was taken up in DMF and purified by preparative HPLC (basic mode) eluting with 20-35% ACN in water. The fractions containing the desired product were combined and concentrated in vacuo to give the title compound (73 mg, 46%). 1H NMR (500 MHz, DMSO-d6) δ ppm 1.22-1.32 (m, 3 H), 3.80 (br s, 3 H), 5.58 (quin, J=6.71 Hz, 1 H), 6.31 (d, J=6.83 Hz, 1 H), 6.48 (br s, 2 H), 6.52-6.63 (m, 5 H), 6.66 (d, J=7.81 Hz, 1 H), 7.52 (d, J=6.35 Hz, 1 H), 7.72 (d, J=2.93 Hz, 1 H), 7.80 (s, 1 H); ESI-MS m/z [M+H]+ calc'd for C20H19N9O, 402; found 402.

後処理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in MeOH (10 mL)
  3. additionPd/C (10%, 700 mg) was added
  4. temperaturethe reaction mixture was maintained under an atmosphere of hydrogen for 30 minutes
  5. filtrationThe mixture was filtered through Celite
  6. concentrationconcentrated
  7. custompurified by preparative HPLC (basic mode)
  8. washeluting with 20-35% ACN in water
  9. additionThe fractions containing the desired product
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-bd34a423c8034c0eba52f025ad0a625a
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835420B2

反応ノート

読み込み中…

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