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Water → HCID 57404565, 화합물

HRID 870286
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인쇄 미리보기

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HRID 870286 반응식
[F:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]2[C:10]=1[NH:9][C:8](=[O:11])[CH:7]2[C:12]1[N:17]=[C:16]([O:18][CH3:19])[N:15]=[C:14]([CH3:20])[N:13]=1.CN1C=CN=C1.[F:27][CH:28]([F:33])[S:29](Cl)(=[O:31])=[O:30].O>ClCCl>[F:27][CH:28]([F:33])[S:29]([N:9]1[C:10]2[C:6](=[CH:5][CH:4]=[CH:3][C:2]=2[F:1])[CH:7]([C:12]2[N:17]=[C:16]([O:18][CH3:19])[N:15]=[C:14]([CH3:20])[N:13]=2)[C:8]1=[O:11])(=[O:31])=[O:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 13901-Methylimidazole2회HCID 73932Difluoromethanesulphonyl chloride2회HCID 867067347-fluoro-3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1,3-dihydro-2H-indol-2-one

생성물 1

HCID 57404565HCID 57404565, 화합물

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

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온도
0 °C

실험 절차

7-Fluoro-3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl)-1,3-dihydro-2H-indol-2-one (1.20 g) and 1-methyl-1H-imidazole (0.97 g) are introduced as initial charge in 10 ml of dichloromethane and cooled to 0° C. under nitrogen. With stirring, difluoromethanesulfonyl chloride (1.21 g) is added in 2 portions and the mixture is warmed to room temperature. After 5 hours, 1-methyl-1H-imidazole (0.32 g) and difluoromethanesulfonyl chloride (0.61 g) are added and the mixture is stirred for 16 hours. After adding water and some hydrochloric acid, the solid is filtered off, washed with dichloromethane and water and dried. This gives the title compound as a solid in an HPLC purity of 91% (1.54 g, 92% of theory). The UV absorption (maximum at 360 nm) verifies the N-sulfonylation of the product.

후처리

  1. temperaturethe mixture is warmed to room temperature
  2. stirringthe mixture is stirred for 16 hours
  3. filtrationsome hydrochloric acid, the solid is filtered off
  4. washwashed with dichloromethane and water
  5. customdried

출처 및 근거

ORD 기록
ord-be3e47d2f4dc4fa6ab98093614bbef3b
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969553B2

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