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Sodium Iodide → 1-cyclohexylmethyl-3-(5-diethylaminomethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole

HRID 644048
ノート
印刷プレビュー

反応式

HRID 644048 の反応式
[CH:1]1([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[O:17][CH3:18])[C:10]([C:19]3[S:20][C:21]([CH2:25]OS(C)(=O)=O)=[C:22]([CH3:24])[N:23]=3)=[CH:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[I-].[Na+].[CH2:39]([NH:41][CH2:42][CH3:43])[CH3:40]>C1COCC1.C(#N)C>[CH:1]1([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][C:15]=3[O:17][CH3:18])[C:10]([C:19]3[S:20][C:21]([CH2:25][N:41]([CH2:42][CH3:43])[CH2:39][CH3:40])=[C:22]([CH3:24])[N:23]=3)=[CH:9]2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]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 5238Sodium IodideHCID 8021DiethylamineHCID 11430Potassium CarbonateHCID 866131991-cyclohexylmethyl-3-(5-methanesulfonyloxymethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole

生成物 1

HCID 686957571-cyclohexylmethyl-3-(5-diethylaminomethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole収率 45.7%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 1-cyclohexylmethyl-3-(5-ethoxycarbonyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (680 mg, 1.65 mmol) in THF (20 ml) was added lithium aluminium hydride (125 mg, 3.30 mmol) at 0° C. The mixture was stirred at 0° C. for 1 h, then quenched with ice water and extracted with dichloromethane. The combined organic layers were washed with brine, dried over sodium sulfate and concentrated. The residue was purified by flash chromatography eluting with 25-50% (v/v) ethyl acetate in heptane then 10% (v/v) methanol in dichloromethane to afford 1-cyclohexylmethyl-3-(5-hydroxymethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (532 mg, 1.44 mmol). To a solution of 1-cyclohexylmethyl-3-(5-hydroxymethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (74 mg, 0.20 mmol) and triethylamine (26 mg, 0.26 mmol) in dichloromethane (1.0 ml), was added methanesulfonyl chloride (28 mg, 0.24 mmol). The mixture was stirred at room temperature for 40 min. and partitioned between dichloromethane and 5% aqueous sodium hydrogen carbonate. The aqueous layer was extracted with dichloromethane, then combined organic layers were washed with brine, dried over sodium sulfate and concentrated to afford crude 1-cyclohexylmethyl-3-(5-methanesulfonyloxymethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (65 mg, 0.15 mmol). A mixture of crude 1-cyclohexylmethyl-3-(5-methanesulfonyloxymethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (64 mg, 0.14 mmol), potassium carbonate (29 mg, 0.21 mmol), sodium iodide (31 mg, 0.21 mmol) and diethylamine (21 mg, 0.28 mmol) in THF (1.5 ml) and acetonitrile (1.5 ml) was subjected to microwave irradiation for 5 min at 160° C. The resulting mixture was partitioned between dichloromethane and water. The aqueous layer was extracted with dichloromethane and combined organic layers were washed with brine, dried over sodium sulfate and concentrated. The residue was purified by flash chromatography eluting with 50-100% (v/v) ethyl acetate in heptane to afford 1-cyclohexylmethyl-3-(5-diethylaminomethyl-4-methylthiazol-2-yl)-7-methoxy-1H-indole (27 mg, 0.064 mmol). Hydrochloride salt formation was achieved by the addition of hydrogen chloride (1M solution in diethyl ether; 1 ml) to a solution of the free base in diethyl ether (1 ml) and ethanol (2 ml). The solvent was removed in vacuo and the precipitate was dried to afford title compound as a 1:1 hydrochloride salt (26 mg, 0.056 mmol). 1H NMR (400 MHz, DMSO-d6) δ 0.95-1.25 (5H, m), 1.29 (6H, t, J 7.2), 1.40-1.52 (2H, m), 1.55-1.70 (3H, m), 1.72-1.84 (1H, m), 3.10-3.25 (4H, m), 3.93 (3H, s), 4.27 (2H, d, J 7.0), 4.56 (2H, d, J 5.0), 6.82 (1H, d, J 7.6), 7.14 (1H, t, J 7.6), 7.72 (1H, d, J 7.6), 8.00 (1H, s), 9.90 (1H, br s); EsIMS: m/z 426.3 [M+H]+, 353.1.

後処理

  1. customirradiation for 5 min at 160° C
  2. customThe resulting mixture was partitioned between dichloromethane and water
  3. extractionThe aqueous layer was extracted with dichloromethane
  4. washwere washed with brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by flash chromatography
  8. washeluting with 50-100% (v/v) ethyl acetate in heptane

出典と根拠

ORDレコード
ord-e2d5fc7087bf4f6dad566969750ef6eb
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700634B2

反応ノート

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