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Diisopropylethylamine → HCID 70645119、化合物

HRID 473973
ノート
印刷プレビュー

反応式

HRID 473973 の反応式
C(N(C(C)C)C(C)C)C.[CH3:10][C:11]([CH3:43])([CH2:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[CH:32]=[C:31]3[C:26]([C:27]([C:34](=[O:42])[NH:35][C:36]4[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=4)=[CH:28][C:29]([CH3:33])=[N:30]3)=[CH:25][CH:24]=2)=[CH:19][N:18]=1)[C:12](O)=[O:13].Br.[N:45]1[NH:46][N:47]=[N:48][C:49]=1[CH2:50][NH2:51].F[P-](F)(F)(F)(F)F.N1(O[P+](N2CCCC2)(N2CCCC2)N2CCCC2)C2C=CC=CC=2N=N1>CN(C)C=O>[N:45]1[NH:46][N:47]=[N:48][C:49]=1[CH2:50][NH:51][C:12](=[O:13])[C:11]([CH3:10])([CH3:43])[CH2:15][O:16][C:17]1[N:18]=[CH:19][C:20]([C:23]2[CH:32]=[C:31]3[C:26]([C:27]([C:34]([NH:35][C:36]4[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=4)=[O:42])=[CH:28][C:29]([CH3:33])=[N:30]3)=[CH:25][CH:24]=2)=[CH:21][CH:22]=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 4

HCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 46926794HCID 46926794、化合物HCID 53444401HCID 53444401、化合物

生成物 1

HCID 70645119HCID 70645119、化合物収率 65%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

N-Ethyl-N,N-diisopropylamine (50.0 μL, 0.300 mmol) was added at room temperature to a solution of 2,2-dimethyl-3-(5-(2-methyl-4-(phenylcarbamoyl)quinolin-7-yl)pyridin-2-yloxy)propanoic acid B-17 (45.5 mg, 0.10 mmol), (2H-tetrazol-5-yl)methanamine hydrobromide (27.7 mg, 0.154 mmol) and (benzotriazol-1-yloxy)tripyrrolidinophosphonium hexafluorophosphate (64.0 mg, 0.123 mmol) in anhydrous N,N-dimethylformamide (5.0 mL) under an atmosphere of nitrogen. The reaction mixture was stirred overnight, then partitioned between methylene chloride (30 mL) and an aqueous solution of pH 7 phosphate buffer (30 mL). The aqueous layer was extracted with methylene chloride (3×30 mL); the combined extracts were successively washed with water (30 mL), brine (30 mL), then dried over anhydrous magnesium sulfate, filtered and concentrated to dryness under reduced pressure. The crude residue was purified by flash column chromatography on silica gel (hexanes:ethyl acetate gradient) to give 7-(6-(3-((2H-tetrazol-5-yl)methylamino)-2,2-dimethyl-3-oxopropoxy)pyridin-3-yl)-2-methyl-N-phenylquinoline-4-carboxamide B-24 (34.9 mg, Yield=65%). 1H NMR (500 MHz, CHLOROFORM-d) δ ppm 1.35 (s, 6H), 2.77 (s, 3H), 3.71-3.74 (m, 2H), 4.75 (d, J=5.5 Hz, 2H), 6.86 (d, J=8.5 Hz, 1H), 7.23-7.30 (m, 2H), 7.45 (t, J=6.5 Hz, 3H), 7.87 (d, J=8.0 Hz, 2H), 7.87 (d, J=8.5 Hz, 1H), 8.24 (d, J=8.5 Hz, 1H), 8.47 (s, 1H), 8.45 (d, J=9.5 Hz, 1H), 8.59 (s, 1H); MS (ESI) [M+1]+ 537.

後処理

  1. custompartitioned between methylene chloride (30 mL)
  2. extractionThe aqueous layer was extracted with methylene chloride (3×30 mL)
  3. washthe combined extracts were successively washed with water (30 mL), brine (30 mL)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure
  7. customThe crude residue was purified by flash column chromatography on silica gel (hexanes:ethyl acetate gradient)

出典と根拠

ORDレコード
ord-0674a8d3f1d240d482bbcbaa4bff8ac5
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08637507B2

反応ノート

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