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Triethylamine → N-(3-(2-chlorothieno[3,2-d]pyrimidin-7-yl)phenyl)methanesulfonamide

HRID 2042209
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HRID 2042209 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[S:10][CH:9]=[C:8]([C:11]3[CH:12]=[C:13]([NH2:17])[CH:14]=[CH:15][CH:16]=3)[C:6]=2[N:7]=1.[CH3:18][S:19](Cl)(=[O:21])=[O:20].C(N(CC)CC)C>O1CCCC1.C(OCC)(=O)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[S:10][CH:9]=[C:8]([C:11]3[CH:12]=[C:13]([NH:17][S:19]([CH3:18])(=[O:21])=[O:20])[CH:14]=[CH:15][CH:16]=3)[C:6]=2[N:7]=1
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참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 866732143-(2-Chlorothieno[3,2-d]pyrimidin-7-yl)benzenamine

생성물 1

HCID 86673215N-(3-(2-chlorothieno[3,2-d]pyrimidin-7-yl)phenyl)methanesulfonamide수율 91.4%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매
HCID 8857
Ethyl Acetate
용매

실험 절차

3-(2-Chlorothieno[3,2-d]pyrimidin-7-yl)benzenamine (800 mg, 3.06 mmol) was dissolved in anhydrous tetrahydrofuran (15 mL) and methanesulfonyl chloride (0.27 mL, 3.37 mmol) and triethylamine (0.85 mL, 6.13 mmol) were added. The mixture solution was stirred for 2 hours, diluted with ethyl acetate, and then washed with brine. The organic layer was concentrated by drying with magnesium sulfate. Purification by chromatography (10% ethyl acetate/hexane) yielded the target compound (950 mg, 91% yield).

후처리

  1. washwashed with brine
  2. concentrationThe organic layer was concentrated
  3. dry with materialby drying with magnesium sulfate
  4. customPurification by chromatography (10% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-5f959c3db4604ab78d4bd3f8a882c3a4
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586580B2

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