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Dichloromethane → (racemic) N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-6-(1-hydroxyethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

HRID 1777994
ノート
印刷プレビュー

反応式

HRID 1777994 の反応式
F.N1C=CC=CC=1.[Si]([O:15][CH:16]([C:18]1[CH:19]=[C:20]2[C:25](=[N:26][C:27]=1[CH:28]([O:31][CH3:32])[O:29][CH3:30])[N:24]([C:33]([NH:35][C:36]1[CH:41]=[C:40]([NH:42][CH2:43][CH2:44][O:45][CH3:46])[C:39]([C:47]#[N:48])=[CH:38][N:37]=1)=[O:34])[CH2:23][CH2:22][CH2:21]2)[CH3:17])(C(C)(C)C)(C)C.C([O-])(O)=O.[Na+].C(Cl)Cl>C1COCC1>[C:47]([C:39]1[C:40]([NH:42][CH2:43][CH2:44][O:45][CH3:46])=[CH:41][C:36]([NH:35][C:33]([N:24]2[C:25]3[C:20](=[CH:19][C:18]([CH:16]([OH:15])[CH3:17])=[C:27]([CH:28]([O:31][CH3:32])[O:29][CH3:30])[N:26]=3)[CH2:21][CH2:22][CH2:23]2)=[O:34])=[N:37][CH:38]=1)#[N:48]
参加物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 6344DichloromethaneHCID 64774Pyridine, hydrofluoride (1:1)HCID 516892Sodium BicarbonateHCID 131734796(racemic) 6-(1-((tert-butyldimethylsilyl)oxy)ethyl)-N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide2 回

生成物 1

HCID 118036612
(racemic) N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-6-(1-hydroxyethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Pyridine hydrofluoride (0.130 ml, 1.012 mmol) was added to a suspension of (racemic) 6-(1-((tert-butyldimethylsilyl)oxy)ethyl)-N-(5-cyano-4-((2-methoxyethyl)amino)pyridin-2-yl)-7-(dimethoxymethyl)-3,4-dihydro-1,8-naphthyridine-1(2H)-carboxamide (intermediate 184, 296 mg, 0.506 mmol) in THF (2.5 ml) and stirred for 18 h. The reaction mixture was poured into saturated aqueous NaHCO3 and DCM was added. Phases were separated and the water phase was back extracted with DCM (3×). Organic phases were combined, dried using Na2SO4, filtered and concentrated. The crude product was purified using silica gel column chromatography eluting with MeOH (0-4%) in DCM to yield the title compound as a colorless solid. (UPLC-MS 3) tR 0.90 min, ESI-MS 471.2 [M+H]+. 1H NMR (600 MHz, DMSO-d6) δ 13.62 (s, 1H), 8.27 (s, 1H), 7.84 (s, 1H), 7.53 (s, 1H), 6.92 (t, 1H), 5.45 (s, 1H), 5.23-5.16 (m, 2H), 3.98-3.88 (m, 2H), 3.53 (t, 2H), 3.41-3.31 (m, 8H), 3.30 (s, 3H), 2.89-2.83 (m, 2H), 1.95-1.86 (m, 2H), 1.30 (d, 3H).

後処理

  1. additionwas added
  2. customPhases were separated
  3. extractionthe water phase was back extracted with DCM (3×)
  4. customdried
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified
  8. washeluting with MeOH (0-4%) in DCM

出典と根拠

ORDレコード
ord-482fb60b4f85448194254ae78ed9b3b5
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09266883B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート