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Triethylamine → Methanesulfonic acid 6-[3-(5-Methylisoxazol-3-yl)-[1,2,4]triazolo[3,4-alpha]-phthalazin-6-yloxymethyl]pyridin-3-ylmethyl ester

HRID 2183496
ノート
印刷プレビュー

反応式

HRID 2183496 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][C:7]1[O:11][N:10]=[C:9]([C:12]2[N:16]3[N:17]=[C:18]([O:25][CH2:26][C:27]4[N:32]=[CH:31][C:30]([CH2:33][OH:34])=[CH:29][CH:28]=4)[C:19]4[C:24]([C:15]3=[N:14][N:13]=2)=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:8]=1.CCN(CC)CC>C(Cl)Cl>[CH3:6][C:7]1[O:11][N:10]=[C:9]([C:12]2[N:16]3[N:17]=[C:18]([O:25][CH2:26][C:27]4[N:32]=[CH:31][C:30]([CH2:33][O:34][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:29][CH:28]=4)[C:19]4[C:24]([C:15]3=[N:14][N:13]=2)=[CH:23][CH:22]=[CH:21][CH:20]=4)[CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 131724934{6-[3-(5-Methylisoxazol-3-yl)-[1,2,4]triazolo[3,4-alpha]phthalazin-6-yloxymethyl]pyridin-3-yl}methanol

生成物 1

HCID 131724935Methanesulfonic acid 6-[3-(5-Methylisoxazol-3-yl)-[1,2,4]triazolo[3,4-alpha]-phthalazin-6-yloxymethyl]pyridin-3-ylmethyl ester

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

Methanesulfonyl chloride (1.07 ml, 13.9 mmol) was added to a stirred suspension of {6-[3-(5-methylisoxazol-3-yl)-[1,2,4]triazolo[3,4-α]phthalazin-6-yloxymethyl]pyridin-3-yl}methanol (2.78 mmol), Et3N (1.94 ml, 13.9 mmol) in CH2Cl2 (100 ml) under nitrogen. The reaction mixture was stirred overnight and then diluted with CH2Cl2. The resulting solution was washed with H2O (100 ml), 1 N HCl (100 ml), NaHCO3 (sat., 100 ml) and brine (100 ml). The solution was then dried MgSO4) and concentrated under reduced pressure. The resultant mesylate was used without further purification.

後処理

  1. washThe resulting solution was washed with H2O (100 ml), 1 N HCl (100 ml), NaHCO3 (sat., 100 ml) and brine (100 ml)
  2. concentrationdried MgSO4) and concentrated under reduced pressure
  3. customThe resultant mesylate was used without further purification

出典と根拠

ORDレコード
ord-389b86a5bb6049b69e8581c4c7b175e0
出典データセット
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06900209B2

反応ノート

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