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Lithium Hexamethyldisilazide → (S)-7-(2-fluoropyridin-3-yl)-3-((R)-3-fluoropyrrolidin-1-yl)-2',6'-dihydrospiro[chromeno [2,3-b]pyridine-5,3'-[1,4]oxazin]-5'-amine

HRID 1472457
ノート
印刷プレビュー

反応式

HRID 1472457 の反応式
Cl.[F:2][C@@H:3]1[CH2:7][CH2:6][NH:5][CH2:4]1.Br[C:9]1[CH:10]=[C:11]2[C@@:22]3([N:27]=[C:26]([NH2:28])[CH2:25][O:24][CH2:23]3)[C:21]3[C:16](=[CH:17][CH:18]=[C:19]([C:29]4[C:30]([F:35])=[N:31][CH:32]=[CH:33][CH:34]=4)[CH:20]=3)[O:15][C:12]2=[N:13][CH:14]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C>CC(OC1C=CC=C(OC(C)C)C=1C1C(P(C2CCCCC2)C2CCCCC2)=CC=CC=1)C.CC(OC)(C)C.C1C=[C-]C(CCN)=CC=1.Cl[Pd+].C1COCC1>[F:35][C:30]1[C:29]([C:19]2[CH:20]=[C:21]3[C@:22]4([N:27]=[C:26]([NH2:28])[CH2:25][O:24][CH2:23]4)[C:11]4[C:12](=[N:13][CH:14]=[C:9]([N:5]5[CH2:6][CH2:7][C@@H:3]([F:2])[CH2:4]5)[CH:10]=4)[O:15][C:16]3=[CH:17][CH:18]=2)=[CH:34][CH:33]=[CH:32][N:31]=1
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 3

HCID 2733832Lithium Hexamethyldisilazide2 回HCID 2759162(3R)-3-fluoropyrrolidine hydrochlorideHCID 67436956(S)-3-bromo-7-(2-fluoropyridin-3-yl)-2',6'-dihydrospiro[chromeno[2,3-b]pyridine-5,3'-[1,4]oxazin]-5'-amine

生成物 1

HCID 58465994(S)-7-(2-fluoropyridin-3-yl)-3-((R)-3-fluoropyrrolidin-1-yl)-2',6'-dihydrospiro[chromeno [2,3-b]pyridine-5,3'-[1,4]oxazin]-5'-amine収率 35.4%

試薬・触媒・溶媒 2

HCID 66572931HCID 66572931、化合物触媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

A vial was charged with 2-fluoropyridin-3-ylboronic acid (0.094 g, 0.667 mmol), PdCl2(dppf)-CH2Cl2-adduct (0.026 g, 0.032 mmol), (S)-3-bromo-7-iodo-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.300 g, 0.635 mmol), and potassium carbonate (0.351 g, 2.54 mmol). Dioxane (3.5 mL) and water (1.5 mL) were added. The vial was flushed with argon, sealed and heated to 80° C. for 1 hour. The reaction mixture was then diluted with EtOAc, dried over MgSO4 and concentrated. Purification of the crude residue by column chromatography [0-80% (90:10:1 DCM/MeOH/NH4OH)/DCM] gave (S)-3-bromo-7-(2-fluoropyridin-3-yl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.202 g, 0.458 mmol) Step 2: A vial was charged with (R)-3-fluoropyrrolidine HCl (0.021 g, 0.170 mmol), (S)-3-bromo-7-(2-fluoropyridin-3-yl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.050 g, 0.113 mmol) and RuPhos palladacycle (9.05 mg, 0.011 mmol). THF (1 mL) and LiHMDS (1N in THF; 0.567 mL, 0.567 mmol) were added, and the reaction mixture was allowed to stir at RT overnight. Additional RuPhos palladacycle (9.05 mg, 0.011 mmol) and LiHMDS solution (0.567 mL, 0.567 mmol) were added, and the reaction mixture was heated to 45° C. for 2 hours. The reaction mixture was then quenched with MeOH and concentrated under reduced pressure. Purification of the crude residue by column chromatography [0-100% (90:10:1 DCM/MeOH/NH4OH)/DCM] gave (S)-7-(2-fluoropyridin-3-yl)-3-((R)-3-fluoropyrrolidin-1-yl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.018 g, 0.040 mmol, 35.3% yield).

後処理

  1. temperaturethe reaction mixture was heated to 45° C. for 2 hours
  2. customThe reaction mixture was then quenched with MeOH
  3. concentrationconcentrated under reduced pressure
  4. customPurification of the crude residue by column chromatography [0-100% (90:10:1 DCM/MeOH/NH4OH)/DCM]

出典と根拠

ORDレコード
ord-ac2946db4b2f42209933882898084864
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09012446B2

反応ノート

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