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Triethylamine → (R)-1-cyclopropyl-3-(3-fluoro-4-(4-(3-methylmorpholino)-6-(methylsulfonyl)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-yl)phenyl)urea

HRID 1626714
ノート
印刷プレビュー

反応式

HRID 1626714 の反応式
Cl.[CH:2]1([NH:5][C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[N:16]=[C:17]([N:24]4[CH2:29][CH2:28][O:27][CH2:26][C@H:25]4[CH3:30])[C:18]4[CH2:23][NH:22][CH2:21][C:19]=4[N:20]=3)=[C:11]([F:31])[CH:10]=2)=[O:7])[CH2:4][CH2:3]1.CCN(CC)CC.[CH3:39][S:40](Cl)(=[O:42])=[O:41]>CN(C=O)C>[CH:2]1([NH:5][C:6]([NH:8][C:9]2[CH:14]=[CH:13][C:12]([C:15]3[N:16]=[C:17]([N:24]4[CH2:29][CH2:28][O:27][CH2:26][C@H:25]4[CH3:30])[C:18]4[CH2:23][N:22]([S:40]([CH3:39])(=[O:42])=[O:41])[CH2:21][C:19]=4[N:20]=3)=[C:11]([F:31])[CH:10]=2)=[O:7])[CH2:3][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 66687170(R)-1-cyclopropyl-3-(3-fluoro-4-(4-(3-methylmorpholino)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-yl)phenyl)urea hydrochloride2 回

生成物 1

HCID 66678989(R)-1-cyclopropyl-3-(3-fluoro-4-(4-(3-methylmorpholino)-6-(methylsulfonyl)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-yl)phenyl)urea収率 24%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a stirring solution of (R)-1-cyclopropyl-3-(3-fluoro-4-(4-(3-methylmorpholino)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-2-yl)phenyl)urea hydrochloride (intermediate 33) (112 mg, 0.25 mmol) in DMF (2 mL) was added NEt3 (70 μl, 0.5 mmol), and methanesulfonyl chloride (21 μL, 0.275 mmol). Reaction was stirred at room temp overnight. The reaction mixture was concentrated in vacuo before partitioning between DCM (10 ml) and water (10 ml). The organic layer was recovered, passed through a hydrophobic frit and the solvent removed in vacuo. Residue was then purified by prep. HPLC at high pH to afford the compound title compound as a light brown solid (30 mg, 0.06 mmol, 24%).

後処理

  1. customReaction
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. custombefore partitioning between DCM (10 ml) and water (10 ml)
  4. customThe organic layer was recovered
  5. customthe solvent removed in vacuo
  6. customResidue was then purified by prep

出典と根拠

ORDレコード
ord-18998d81538d4d6e9c570c15bb1fc051
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785457B2

反応ノート

読み込み中…

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