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4-Methylmorpholine → HCID 178448521、化合物

HRID 468640
ノート
印刷プレビュー

反応式

HRID 468640 の反応式
CN1CCOCC1.[F:8][C:9]1[C:10]([C:27]2[CH:32]=[CH:31][C:30]([O:33][CH2:34][C@H:35]3[CH2:40][CH2:39][C@H:38]([O:41][CH:42]4[CH2:47][CH2:46][CH2:45][CH2:44][O:43]4)[CH2:37][CH2:36]3)=[CH:29][CH:28]=2)=[CH:11][C:12](=[O:26])[N:13]([CH2:15][CH2:16][C@@:17]([CH3:25])([S:21]([CH3:24])(=[O:23])=[O:22])[C:18](O)=[O:19])[CH:14]=1.ClC1N=C(OC)N=C(OC)N=1.[O:59]1[CH2:64][CH2:63][CH2:62][CH2:61][CH:60]1[O:65][NH2:66]>CC1CCCO1.O>[F:8][C:9]1[C:10]([C:27]2[CH:28]=[CH:29][C:30]([O:33][CH2:34][C@H:35]3[CH2:40][CH2:39][C@H:38]([O:41][CH:42]4[CH2:47][CH2:46][CH2:45][CH2:44][O:43]4)[CH2:37][CH2:36]3)=[CH:31][CH:32]=2)=[CH:11][C:12](=[O:26])[N:13]([CH2:15][CH2:16][C@@:17]([CH3:25])([S:21]([CH3:24])(=[O:23])=[O:22])[C:18]([NH:66][O:65][CH:60]2[CH2:61][CH2:62][CH2:63][CH2:64][O:59]2)=[O:19])[CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 184502-Chloro-4,6-dimethoxy-1,3,5-triazineHCID 5142091O-(Tetrahydropyran-2-yl)hydroxylamineHCID 178448522HCID 178448522、化合物

生成物 1

HCID 178448521HCID 178448521、化合物

試薬・触媒・溶媒 2

HCID 962Water
溶媒
HCID 73012-Methyltetrahydrofuran溶媒

実験手順

N-Methyl morpholine (340 uL, 3.09 mmol) was added to a suspension of (2R)-4-[5-fluoro-2-oxo-4-(4-{[trans-4-(tetrahydro-2H-pyran-2-yloxy)cyclohexyl]methoxy}-phenyl)pyridin-1(2H)-yl]-2-methyl-2-(methylsulfonyl)butanoic acid (1.28 g, 2.21 mmol), 2-chloro-4,6-dimethoxy-1,3,5-triazine (510 mg, 2.87 mmol) in 2-methyltetrahydrofuran (30 mL) and the reaction was stirred for 1 h at rt. O-(Tetrahydro-2H-pyran-2-yl)hydroxylamine (61 mg, 0.52 mmol) was added, and the reaction was stirred overnight at rt. Water (50 mL) was added, and the mixture was extracted with EtOAc (3×150 mL). The combined organic phases were dried (Na2SO4), filtered, and concentrated under reduced pressure. The crude material was purified via flash chromatography using an eluent of EtOAc in n-heptane (75-100%) to afford the title compound as a light brown residue (700 mg, 46%). MS (LCMS) m/z 677.4 (M+1).

後処理

  1. stirringthe reaction was stirred overnight at rt
  2. extractionthe mixture was extracted with EtOAc (3×150 mL)
  3. dry with materialThe combined organic phases were dried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe crude material was purified via flash chromatography

出典と根拠

ORDレコード
ord-bdfc5ed945bb43c3bb32c9789fc41c00
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08624034B2

反応ノート

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