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1,2-Dichloroethane → N-[(1S,2S)-2-{[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]amino}cyclopentyl]-5-fluoro-2-(pyrimidin-2-yl)benzamide

HRID 1750716
ノート
印刷プレビュー

反応式

HRID 1750716 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[C:6]([CH:10]=1)[C:7]([OH:9])=O.N1C2C(=NC=CC=2)N(O)N=1.C(Cl)CCl.C(N(CC)CC)C.Cl.[CH2:39]([C:41]1[C:42]([NH:51][C@H:52]2[CH2:56][CH2:55][CH2:54][C@@H:53]2[NH2:57])=[N:43][CH:44]=[C:45]([C:47]([F:50])([F:49])[F:48])[N:46]=1)[CH3:40]>C(Cl)Cl>[CH2:39]([C:41]1[C:42]([NH:51][C@H:52]2[CH2:56][CH2:55][CH2:54][C@@H:53]2[NH:57][C:7](=[O:9])[C:6]2[CH:10]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=2[C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[N:43][CH:44]=[C:45]([C:47]([F:50])([F:48])[F:49])[N:46]=1)[CH3:40]
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 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 181649HOAtHCID 670869505-Fluoro-2-(pyrimidin-2-yl)benzoic acidHCID 118308132(1S,2S)-1-N-[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]cyclopentane-1,2-diamine hydrochloride2 回

生成物 1

HCID 91827608
N-[(1S,2S)-2-{[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]amino}cyclopentyl]-5-fluoro-2-(pyrimidin-2-yl)benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-fluoro-2-(pyrimidin-2-yl)benzoic acid (CAS number 1293284-57-7; 53 mg, 0.24 mmol), 3H-[1,2,3]triazolo[4,5-b]pyridin-3-ol (33 mg, 0.24 mmol), EDC (46.3 mg, 0.241 mmol) and triethylamine (0.067 ml, 0.48 mmol) in DCM (5 ml) was added (1S,2S)-1-N-[3-ethyl-5-(trifluoromethyl)pyrazin-2-yl]cyclopentane-1,2-diamine hydrochloride (Intermediate 41; 50 mg, 0.161 mmol). The reaction mixture was stirred at room temperature for 88 hours and then partitioned between DCM and a saturated solution of sodium bicarbonate, passing through a hydrophobic frit. The organics were loaded directly on to a cation/anion mixed mode cartridge, eluted with DCM and concentrated in vacuo. This was then purified by reverse phase chromatography (C18 silica, 0-100% acetonitrile/water with 0.1% ammonia). The resulting aqueous was concentrated in vacuo and extracted with DCM. The organics were concentrated in vacuo to afford the title compound.

後処理

  1. custompartitioned between DCM
  2. additionmixed mode cartridge
  3. washeluted with DCM
  4. concentrationconcentrated in vacuo
  5. customThis was then purified by reverse phase chromatography (C18 silica, 0-100% acetonitrile/water with 0.1% ammonia)
  6. concentrationThe resulting aqueous was concentrated in vacuo
  7. extractionextracted with DCM
  8. concentrationThe organics were concentrated in vacuo

出典と根拠

ORDレコード
ord-c3375234c59d46b38d9fa1a892e22a3f
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156829B2

反応ノート

読み込み中…

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