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Nitrogen → 1-(Tert-butoxycarbonyl)indole

HRID 2078687
ノート
印刷プレビュー

反応式

HRID 2078687 の反応式
[C:1]([O:5][C:6]([N:8]1[C:12]2[CH:13]=[CH:14]S[C:11]=2[C:10](I)=N1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[C:17](=O)([O-])[O-].[K+].[K+].N#N.O1CC[CH2:27][CH2:26]1>C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[C:1]([O:5][C:6]([N:8]1[C:12]2[C:11](=[CH:10][CH:17]=[CH:14][CH:13]=2)[CH:27]=[CH:26]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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

7

反応物 4

HCID 947NitrogenHCID 8028TetrahydrofuranHCID 11430Potassium CarbonateHCID 57637299tert-Butyl 3-iodo-1H-thieno[3,2-c]pyrazole-1-carboxylate

生成物 1

HCID 35329801-(Tert-butoxycarbonyl)indole収率 69%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
57.5 °C

実験手順

A mixture of 5-(tert-butyl-dimethyl-silanyloxymethyl)-1H-indole-2-boronic acid 1-carboxylic acid tert-butyl ester [3.82 g, 9.42 mmol, Intermediate (8), prepared as described in Example 1-4 of International Patent Application Publication No. WO 02/32861], 3-iodo-thieno[3,2-c]pyrazole-1-carboxylic acid tert-butyl ester [4.0 g, 11.42 mmol, Example 5B above], tetrakis(triphenylphosphine)palladium(0) (544 mg, 0.470 mmol), potassium carbonate (2M aqueous, 12 mL) in tetrahydrofuran (60 mL) is purged with N2 for 10 minutes then heated to 55-60° C. for 7.5 hours. The reaction is diluted with ethyl acetate (50 mL) and washed with water (20 mL). Water layer is back extracted with ethyl acetate (50 mL). The combined ethyl acetate phases are dried over sodium sulfate. The residue is chromatographed on 35 g silica gel cartridge (5-30% ethyl acetate gradient in heptane) to give 2-(1-tert-butoxycarbonyl-1H-thieno[3,2-c]pyrazol-3-yl)-5-tert-butyl-dimethyl-silanyloxymethyl)-indole-1-carboxlic acid tert-butyl ester [3.8 g, 69%, Intermediate (9)]; 1H NMR [(CD3)2SO)]: δ 8.08 (2H, m), 7.64 (1H, s), 7.38 (2H, m), 7.14 (1H, s), 4.81 (2H, s, —OCH), 1.65 (9H, s), 1.32 (9H, s), 0.92 (9H, s, Si(CH3)3), 0.10 (6H, s, Si(CH2)); LC/MS: 584 (M+H).

後処理

  1. customprepared
  2. washwashed with water (20 mL)
  3. extractionWater layer is back extracted with ethyl acetate (50 mL)
  4. dry with materialThe combined ethyl acetate phases are dried over sodium sulfate
  5. customThe residue is chromatographed on 35 g silica gel cartridge (5-30% ethyl acetate gradient in heptane)

出典と根拠

ORDレコード
ord-f3188e6a250b42d987308ab3300ed689
出典データセット
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07928231B2

反応ノート

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