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Triethylamine → (R)-(3-methyl-4-(1-phenylpyrido[4,3-d]pyridazin-4-yl)piperazin-1-yl)(tetrahydro-2H-pyran-4-yl)methanone

HRID 1514375
ノート
印刷プレビュー

反応式

HRID 1514375 の反応式
[CH3:1][C@@H:2]1[CH2:7][NH:6][CH2:5][CH2:4][N:3]1[C:8]1[N:9]=[N:10][C:11]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)=[C:12]2[CH:17]=[CH:16][N:15]=[CH:14][C:13]=12.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.C(N(CC)CC)C.[O:52]1[CH2:57][CH2:56][CH:55]([C:58](O)=[O:59])[CH2:54][CH2:53]1.C([O-])(O)=O.[Na+]>ClCCl.C(OCC)(=O)C>[CH3:1][C@H:2]1[N:3]([C:8]2[C:13]3[CH:14]=[N:15][CH:16]=[CH:17][C:12]=3[C:11]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[N:10][N:9]=2)[CH2:4][CH2:5][N:6]([C:58]([CH:55]2[CH2:56][CH2:57][O:52][CH2:53][CH2:54]2)=[O:59])[CH2:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 219302Oxane-4-carboxylic acidHCID 516892Sodium BicarbonateHCID 57657605(R)-4-(2-methylpiperazin-1-yl)-1-phenylpyrido[3,4-d]pyridazine

生成物 1

HCID 25226765
(R)-(3-methyl-4-(1-phenylpyrido[4,3-d]pyridazin-4-yl)piperazin-1-yl)(tetrahydro-2H-pyran-4-yl)methanone

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of (R)-4-(2-methylpiperazin-1-yl)-1-phenylpyrido[4,3-d]pyridazine 16 (125 mg, 409 μmol) in dichloromethane (5 mL) was added HOBT (3.1 mg, 20 μmol), EDCI (86 mg, 450 μmol), triethylamine (114 μl, 819 μmol), and tetrahydro-2H-pyran-4-carboxylic acid (64 mg, 491 μmol). After 1 hour, 10 mL of sat NaHCO3 and 100 mL of ethyl acetate were added. The layers were separated and the organic layer was washed with 1×10 mL of brine, dried over MgSO4, filtered, and concentrated. Purified by column chromatography (hexanes:acetone) to isolate (R)-(3-methyl-4-(1-phenylpyrido[4,3-d]pyridazin-4-yl)piperazin-1-yl)(tetrahydro-2H-pyran-4-yl)methanone 30. MS: 417.2 (calc'd) 418.1 (M+H, found).

後処理

  1. customThe layers were separated
  2. washthe organic layer was washed with 1×10 mL of brine
  3. dry with materialdried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurified by column chromatography (hexanes:acetone)

出典と根拠

ORDレコード
ord-541013da3de34f3393b79f8a2a11665e
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08222251B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート