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Potassium Carbonate → (S)-7-(2-fluoropyridin-3-yl)-3-(neopentyloxy)-2',6'-dihydrospiro[chromeno[2,3-b]pyridine-5,3'-[1,4]oxazin]-5'-amine

HRID 1472423
ノート
印刷プレビュー

反応式

HRID 1472423 の反応式
[NH2:1][C:2]1[CH2:7][O:6][CH2:5][C@:4]2([C:20]3[C:15](=[N:16][CH:17]=[C:18]([OH:21])[CH:19]=3)[O:14][C:13]3[C:8]2=[CH:9][C:10]([C:22]2[C:23]([F:28])=[N:24][CH:25]=[CH:26][CH:27]=2)=[CH:11][CH:12]=3)[N:3]=1.C(=O)([O-])[O-].[K+].[K+].[CH2:35](I)[C:36]([CH3:39])([CH3:38])[CH3:37]>CN(C=O)C.CC1OCCC1>[F:28][C:23]1[C:22]([C:10]2[CH:9]=[C:8]3[C@:4]4([N:3]=[C:2]([NH2:1])[CH2:7][O:6][CH2:5]4)[C:20]4[C:15](=[N:16][CH:17]=[C:18]([O:21][CH2:35][C:36]([CH3:39])([CH3:38])[CH3:37])[CH:19]=4)[O:14][C:13]3=[CH:12][CH:11]=2)=[CH:27][CH:26]=[CH:25][N:24]=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 11430Potassium CarbonateHCID 84953Propane, 1-iodo-2,2-dimethyl-HCID 67437546(S)-5'-amino-7-(2-fluoropyridin-3-yl)-2',6'-dihydrospiro[chromeno[2,3-b]pyridine-5,3'-[1,4]oxazin]-3-ol

生成物 1

HCID 58465959(S)-7-(2-fluoropyridin-3-yl)-3-(neopentyloxy)-2',6'-dihydrospiro[chromeno[2,3-b]pyridine-5,3'-[1,4]oxazin]-5'-amine収率 15.9%

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 73012-Methyltetrahydrofuran溶媒

実験手順

A vial charged with a solution of (S)-3-bromo-7-iodo-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.880 g, 1.864 mmol), 2-fluoropyridin-3-ylboronic acid (0.276 g, 1.957 mmol), PdCl2(dppf)-CH2Cl2-adduct (0.038 g, 0.047 mmol), and potassium carbonate (1.031 g, 7.46 mmol). Dioxane (10 mL) and water (5 mL) were added, and the vial was flushed with argon and heated to 100° C. for 90 minutes. Pd2(dba)3 (0.171 g, 0.186 mmol), di-tert-butyl(2′,4′,6′-triisopropyl-3,4,5,6-tetramethylbiphenyl-2-yl)phosphine (0.224 g, 0.466 mmol), and potassium hydroxide (1.046 g, 18.64 mmol) were added to the reaction mixture. The vial was sealed and heated to 120° C. for an additional 3 hours. The reaction mixture was then neutralized to pH 7 with 1N HCl, and was diluted with 2-MeTHF. The organics were dried over MgSO4 and concentrated. Purification of the crude residue by column chromatography [0-100% (90:10:1 DCM/MeOH/NH4OH)/DCM] gave (S)-5′-amino-7-(2-fluoropyridin-3-yl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-3-ol (0.133 g, 0.352 mmol). Step 2: A solution of (S)-5′-amino-7-(2-fluoropyridin-3-yl)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-3-ol (0.133 g, 0.352 mmol), potassium carbonate (0.194 g, 1.406 mmol), and neopentyl iodide (0.093 mL, 0.703 mmol) in 1.5 mL DMF was heated to 115° C. overnight. The reaction mixture was then diluted with 2-MeTHF and washed with water. The organics were dried over MgSO4 and concentrated. Purification of the crude residue by column chromatography [0-100% (9:1 EtOAc/MeOH)/DCM] gave (S)-7-(2-fluoropyridin-3-yl)-3-(neopentyloxy)-2′,6′-dihydrospiro[chromeno[2,3-b]pyridine-5,3′-[1,4]oxazin]-5′-amine (0.025 g, 0.056 mmol, 15.86% yield). MS m/z=449.20 [M+H]+. Calculated for C25H25FN4O3: 448.49.

後処理

  1. washwashed with water
  2. dry with materialThe organics were dried over MgSO4
  3. concentrationconcentrated
  4. customPurification of the crude residue by column chromatography [0-100% (9:1 EtOAc/MeOH)/DCM]

出典と根拠

ORDレコード
ord-87b0fd3da3534809bacd625dddbefc10
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

読み込み中…

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