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2,3-Dihydroxybutanedioic Acid → 4-{(Isobutyl)-[(isoquinolin-1-yl)-methyl]amino}-piperidine-1-carboxylic acid tert-butyl ester

HRID 2111904
ノート
印刷プレビュー

反応式

HRID 2111904 の反応式
CN(OC)[C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][N:6]=1)=O.[H-].C([Al+]CC(C)C)C(C)C.C(O)(=O)C(C(C(O)=O)O)O.C(=O)(O)[O-].[Na+].[C:42]([O:46][C:47]([N:49]1[CH2:54][CH2:53][CH:52]([NH:55][CH2:56][CH:57]([CH3:59])[CH3:58])[CH2:51][CH2:50]1)=[O:48])([CH3:45])([CH3:44])[CH3:43].C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].[OH-].[Na+]>C1(C)C=CC=CC=1.ClCCCl.C(O)(=O)C>[C:42]([O:46][C:47]([N:49]1[CH2:50][CH2:51][CH:52]([N:55]([CH2:56][CH:57]([CH3:59])[CH3:58])[CH2:3][C:5]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]=[CH:7][N:6]=2)[CH2:53][CH2:54]1)=[O:48])([CH3:45])([CH3:44])[CH3:43]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

11

反応物 7

HCID 8752,3-Dihydroxybutanedioic AcidHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 15380699tert-Butyl 4-(isobutylamino)piperidine-1-carboxylateHCID 21225700Diisobutylaluminumhydride
HCID 58678647
N-methoxy-N-methylisoquinoline-1-carboxamide

生成物 1

HCID 685750224-{(Isobutyl)-[(isoquinolin-1-yl)-methyl]amino}-piperidine-1-carboxylic acid tert-butyl ester収率 16.7%

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 176Acetic Acid溶媒HCID 1140Toluene溶媒2 回

反応条件

温度
-37 °C

実験手順

A mixture of N-methyl N-methoxy isoquinoline-1-carboxamide (0.75 g, 3.47 mmol) in dry toluene (25 ml) is cooled to −37° C. and a solution of diisobutylaluminumhydride (DIBAL-H) in toluene (1M, 3.8 ml) is added. The reaction temperature is slowly increased to −4° C. over 4 h and a 20% aqueous solution of tartaric acid (10 ml) is added. The mixture is stirred for 10 min at ambient temperature, saturated aqueous sodium bicarbonate is added and the mixture extracted with dichloromethane. The combined organic layers are dried over sodium sulfate, filtered, and concentrated. The crude product and 4-(isobutylamino)-piperidine-1-carboxylic acid tert-butyl ester (0.89 g, 3.47 mmol), acetic acid (0.2 ml), and 1,2-dichloroethane (15 ml) are mixed and sodium triacetoxyborohydride (1.03 g, 4.86 mmol) is added. The reaction is stirred at ambient temperature over night. Aqueous sodium hydroxide (2M) is added and the mixture is extracted with diethyl ether. The combined organic layers are dried over sodium sulfate, filtered, and concentrated. The crude product is purified by column chromatography [silica, acetone/hexane (15:85)], followed by [silica, ethyl acetate/hexane (5:95), followed by ethyl acetate/hexane (1:3)] to give 0.23 g of 4-{(isobutyl)-[(isoquinolin-1-yl)-methyl]amino}-piperidine-1-carboxylic acid tert-butyl ester: mass spectrum (ion spray): m/z=398.1 (M+1). 1H NMR (CDCl3): δ=8.60 (1H, d), 8.39 (1H, d), 7.79 (1H, d), 7.65 (1H, dd), 7.53-7.56 (2H, m), 4.10-4.30 (4H, m), 2.50-2.70 (3H, m), 2.25-2.35 (2H, m), 2.80-2.85 (2H, m), 1.45-1.60 (3H, m), 1.46 (9H, s), 0.68 (6H, d).

後処理

  1. temperatureThe reaction temperature is slowly increased to −4° C. over 4 h
  2. extractionthe mixture extracted with dichloromethane
  3. dry with materialThe combined organic layers are dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. stirringThe reaction is stirred at ambient temperature over night
  7. extractionthe mixture is extracted with diethyl ether
  8. dry with materialThe combined organic layers are dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude product is purified by column chromatography [silica, acetone/hexane (15:85)]

出典と根拠

ORDレコード
ord-98b4aa44f8124847bf4c89e4a40f2001
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07521462B2

反応ノート

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