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4-Methylmorpholine → HCID 178425645, 화합물

HRID 351127
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HRID 351127 반응식
Cl.[F:2][C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[CH3:12])[C:6]([NH2:8])=[NH:7].[Cl:13][C:14]1[CH:15]=[C:16]([S:21](Cl)(=[O:23])=[O:22])[CH:17]=[CH:18][C:19]=1[F:20].CN1CCOCC1>C1COCC1>[Cl:13][C:14]1[CH:15]=[C:16]([S:21]([NH:7][C:6](=[NH:8])[C:5]2[CH:9]=[CH:10][C:11]([CH3:12])=[C:3]([F:2])[CH:4]=2)(=[O:22])=[O:23])[CH:17]=[CH:18][C:19]=1[F:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 79724-MethylmorpholineHCID 1452223-Chloro-4-fluorobenzenesulphonyl chlorideHCID 16667439Benzenecarboximidamide, 3-fluoro-4-methyl-, hydrochloride (1:1)

생성물 1

HCID 178425645HCID 178425645, 화합물수율 36%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Add 3-fluoro-4-methylbenzamidine hydrochloride (0.025 g, 0.133 mmol) in THF (0.5 mL) to 3-chloro-4-fluorophenyl sulfonylchloride (0.0304 g, 0.133 mmol) followed by N-methylmorpholine (0.2 mL). The reaction mixture was concentrated and chromatographed using reverse phase chromatography (gradient of 5–95% (0.1% TFA in CH3CN) in (0.1% TFA in H2O). A white solid (16.4 mg, 36%) was isolated. ES Positive Ion MS [M+H]+ ions observed: m/z 345 (35Cl) and m/z 347 (37Cl).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customchromatographed

출처 및 근거

ORD 기록
ord-44a9351510d64d7b92f38cfef0672da9
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07183320B2

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