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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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1,2-Dichloroethane → 1-{[6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)pyridin-2-yl]methyl}-N-methyl-1H-1,2,3-triazole-4-carboxamide

HRID 386043
ノート
印刷プレビュー

反応式

HRID 386043 の反応式
[NH2:1][C:2]([C:4]1[CH:8]=[C:7]([C:9]2[C:14]([F:15])=[CH:13][C:12]([C:16]([OH:19])([CH3:18])[CH3:17])=[CH:11][C:10]=2[F:20])[S:6][C:5]=1[NH:21][C:22]1[N:27]=[C:26]([CH2:28][N:29]2[CH:33]=[C:32]([C:34]([O-])=[O:35])[N:31]=[N:30]2)[CH:25]=[CH:24][CH:23]=1)=[O:3].[K+].C1C=CC2N(O)N=[N:44][C:42]=2C=1.C(Cl)CCl.Cl.CN.CCN(C(C)C)C(C)C>CN(C=O)C.O>[NH2:1][C:2]([C:4]1[CH:8]=[C:7]([C:9]2[C:10]([F:20])=[CH:11][C:12]([C:16]([OH:19])([CH3:17])[CH3:18])=[CH:13][C:14]=2[F:15])[S:6][C:5]=1[NH:21][C:22]1[N:27]=[C:26]([CH2:28][N:29]2[CH:33]=[C:32]([C:34]([NH:44][CH3:42])=[O:35])[N:31]=[N:30]2)[CH:25]=[CH:24][CH:23]=1)=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 6364545Methylamine hydrochlorideHCID 68671625Potassium 1-{[6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)pyridin-2-yl]methyl}-1H-1,2,3-triazole-4-carboxylate

生成物 1

HCID 59526258
1-{[6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)pyridin-2-yl]methyl}-N-methyl-1H-1,2,3-triazole-4-carboxamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Potassium 1-{[6-({3-(aminocarbonyl)-5-[2,6-difluoro-4-(1-hydroxy-1-methylethyl)phenyl]-2-thienyl}amino)pyridin-2-yl]methyl}-1H-1,2,3-triazole-4-carboxylate (111 mg, 0.20 mmol), HOBT (62 mg, 0.40 mmol), EDC (77 mg, 0.40 mmol), and methylamine hydrochloride (41 mg, 0.60 mmol) were combined in DMF (5.0 mL), and DIEA (105 μL, 0.60 mmol) was added. The reaction was stirred at room temperature overnight. The solution was diluted with water to precipitate an off-white solid that was collected by filtration, washed (water, MeOH, CH2Cl2), and dried to yield the title compound. 1H NMR (600 MHz, DMSO-d6) δ 12.15 (s, 1H), 8.55 (s, 1H), 8.30 (q, 1H), 7.86 (s, 1H), 7.73-7.66 (m, 2H), 7.36 (s, 1H), 7.21 (d, 2H), 7.03 (d, 1H), 6.80 (d, 1H), 5.71 (s, 2H), 5.27 (s, 1H), 2.66 (d, 3H), 1.42 (s, 6H). Calc'd for C24H24F2N7O3S [M+H]+ 528. found 528.

後処理

  1. customto precipitate an off-white solid
  2. filtrationthat was collected by filtration
  3. washwashed (water, MeOH, CH2Cl2)
  4. customdried

出典と根拠

ORDレコード
ord-bf71fae2ad134b7391774f78b11f99bd
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367706B2

反応ノート

読み込み中…

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