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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
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반응식

HRID 2183496 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

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반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-389b86a5bb6049b69e8581c4c7b175e0
출처 데이터셋
uspto-grants-2005_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06900209B2

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