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Triethylamine → HCID 67958748、化合物

HRID 72512
ノート
印刷プレビュー

反応式

HRID 72512 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:11]2[CH2:14][CH:13]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:17]=3[F:23])[CH2:12]2)=[C:6]([CH:10]=1)[C:7](O)=[O:8].O.ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C.Cl.[NH2:48][C:49]1([C:52]2[CH:61]=[CH:60][C:55]([C:56]([O:58][CH3:59])=[O:57])=[CH:54][CH:53]=2)[CH2:51][CH2:50]1.C(N(CC)CC)C>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:11]2[CH2:12][CH:13]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([F:22])=[CH:18][C:17]=3[F:23])[CH2:14]2)=[C:6]([CH:10]=1)[C:7]([NH:48][C:49]1([C:52]2[CH:61]=[CH:60][C:55]([C:56]([O:58][CH3:59])=[O:57])=[CH:54][CH:53]=2)[CH2:51][CH2:50]1)=[O:8]
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 8471TriethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 66824369Methyl 4-(1-aminocyclopropyl)benzoate hydrochlorideHCID 679580805-Chloro-2-(3-((2,4-difluorophenyl)amino)azetidin-1-yl)nicotinic acid

生成物 1

HCID 67958748
HCID 67958748、化合物
収率 173.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A mixture of 5-chloro-2-(3-((2,4-difluorophenyl)amino)azetidin-1-yl)nicotinic acid (D118) (40 mg, 0.118 mmol), 1-Hydroxybenzotriazole hydrate (18 mg, 0.118 mmol) and 1-Ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (34 mg, 0.177 mmol) in dimethylformamide (5 ml) was stirred 10 min at room temperature. A solution of methyl 4-(1-aminocyclopropyl)benzoate hydrochloride (D7) (32.2 mg, 0.141 mmol) and triethylamine (0.02 ml, 0.141 mmol) in dry dimethylformamide (2 ml) was added and the mixture was stirred 24 h at room temperature. After solvent evaporation, water (10 ml) was added and the formed precipitate was filtered off and purified by Biotage SNAP-Si (10 g) cartridge eluting with a mixture dichloromethane/methanol from 100/0 to 80/20. Collected fractions, after solvent evaporation afforded the title compound (D169) (105 mg).

後処理

  1. stirringthe mixture was stirred 24 h at room temperature
  2. customAfter solvent evaporation, water (10 ml)
  3. additionwas added
  4. filtrationthe formed precipitate was filtered off
  5. custompurified by Biotage SNAP-Si (10 g) cartridge
  6. washeluting with a mixture dichloromethane/methanol from 100/0 to 80/20
  7. customCollected fractions, after solvent evaporation

出典と根拠

ORDレコード
ord-f9fd8496b8c24567963244c5777053ad
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08828987B2

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