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Diisopropylethylamine → 7-Fluoro-3-methyl-1-[2-(4-{[(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)methyl]amino}piperidin-1-yl)ethyl]quinazoline-2,4(1H,3H)-dione

HRID 1644420
ノート
印刷プレビュー

反応式

HRID 1644420 の反応式
FC(F)(F)C(O)=O.[NH2:8][CH:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][N:17]2[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([F:27])[CH:25]=3)[C:20](=[O:28])[N:19]([CH3:29])[C:18]2=[O:30])[CH2:11][CH2:10]1.C(N(CC)C(C)C)(C)C.[O:40]=[C:41]1[CH2:46][O:45][C:44]2[CH:47]=[CH:48][C:49]([CH:51]=O)=[N:50][C:43]=2[NH:42]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl.O>[F:27][C:24]1[CH:25]=[C:26]2[C:21]([C:20](=[O:28])[N:19]([CH3:29])[C:18](=[O:30])[N:17]2[CH2:16][CH2:15][N:12]2[CH2:11][CH2:10][CH:9]([NH:8][CH2:51][C:49]3[CH:48]=[CH:47][C:44]4[O:45][CH2:46][C:41](=[O:40])[NH:42][C:43]=4[N:50]=3)[CH2:14][CH2:13]2)=[CH:22][CH:23]=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 81531DiisopropylethylamineHCID 5049666Sodium triacetoxyborohydrideHCID 218737373-Oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazine-6-carbaldehydeHCID 667742531-[2-(4-Aminopiperidin-1-yl)ethyl]-7-fluoro-3-methylquinazoline-2,4(1H,3H)-dione trifluoroacetate salt2 回

生成物 1

HCID 15982405
7-Fluoro-3-methyl-1-[2-(4-{[(3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazin-6-yl)methyl]amino}piperidin-1-yl)ethyl]quinazoline-2,4(1H,3H)-dione
収率 21%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒2 回

実験手順

1-[2-(4-Aminopiperidin-1-yl)ethyl]-7-fluoro-3-methylquinazoline-2,4(1H,3H)-dione trifluoroacetate salt (Intermediate 134) (0.476 mmol, 380 mg crude) was converted to the free base with N,N-diisopropylethylamine (0.5 mL, 3.0 mmol) and reacted with 3-oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]oxazine-6-carbaldehyde (WO 2004/058144) (102 mg, 0.571 mmol) and sodium triacetoxy borohydride (222 mg, 1.05 mmol) as described for Example 55. The reaction was diluted with dichloromethane and water. The layers were separated. The aqueous layer was extracted with dichloromethane twice. The combined organic layers were dried over magnesium sulfate and evaporated at reduced pressure. Chromatography on silica gel using methanol in dichloromethane (0-9%) with 1% concentrated ammonium hydroxide (aqueous) gave the product as a waxy material. This material was taken up in dichloromethane and washed well with water. The organic phase was dried over magnesium sulfate and evaporated to obtain the title compound as a colorless solid (48 mg, 21%).

後処理

  1. customThe layers were separated
  2. extractionThe aqueous layer was extracted with dichloromethane twice
  3. dry with materialThe combined organic layers were dried over magnesium sulfate
  4. customevaporated at reduced pressure
  5. customgave the product as a waxy material
  6. washwashed well with water
  7. dry with materialThe organic phase was dried over magnesium sulfate
  8. customevaporated

出典と根拠

ORDレコード
ord-a546f123c6034e949a7e1c3fea956288
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08124602B2

反応ノート

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