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Methane → 3-(5-Chloro-2-methoxybenzamido)-2,2-dimethyl-6-(methylaminothiocarbonylaminosulfonyl)-7-methoxychroman

HRID 1457760
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인쇄 미리보기

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HRID 1457760 반응식
[CH3:1][N:2]=[C:3]=[S:4].[Cl:5][C:6]1[CH:7]=[CH:8][C:9]([O:33][CH3:34])=[C:10]([CH:32]=1)[C:11]([NH:13][CH:14]1[CH2:23][C:22]2[C:17](=[CH:18][C:19]([O:28][CH3:29])=[C:20]([S:24](=[O:27])(=[O:26])[NH2:25])[CH:21]=2)[O:16][C:15]1([CH3:31])[CH3:30])=[O:12].C(=O)([O-])[O-].[K+].[K+].C>CS(C)=O>[Cl:5][C:6]1[CH:7]=[CH:8][C:9]([O:33][CH3:34])=[C:10]([CH:32]=1)[C:11]([NH:13][CH:14]1[CH2:23][C:22]2[C:17](=[CH:18][C:19]([O:28][CH3:29])=[C:20]([S:24]([NH:25][C:3]([NH:2][CH3:1])=[S:4])(=[O:27])=[O:26])[CH:21]=2)[O:16][C:15]1([CH3:31])[CH3:30])=[O:12]
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참가 물질

6

반응물 4

HCID 297MethaneHCID 11167Methyl isothiocyanateHCID 11430Potassium CarbonateHCID 221004413-(5-Chloro-2-methoxybenzamido)-2,2-dimethyl-6-sulfamoyl-7-methoxychroman

생성물 1

HCID 538607243-(5-Chloro-2-methoxybenzamido)-2,2-dimethyl-6-(methylaminothiocarbonylaminosulfonyl)-7-methoxychroman

시약·촉매·용매 1

HCID 679
Dimethyl Sulfoxide
용매

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온도
80 °C

실험 절차

0.26 g (3.5 mmol) of methyl isothiocyanate was added to a suspension of 1.14 g (2.5 mmol) of 3-(5-chloro-2-methoxybenzamido)-2,2-dimethyl-6-sulfamoyl-7-methoxychroman and 1.04 g (7.5 mmol) of finely powdered potassium carbonate in 10 ml of DMSO. After the mixture had been stirred at 80° C. for 25 minutes, it was cooled, introduced into ice/water, clarified with charcoal and acidified to pH 1. The precipitate was filtered off with suction and recrystallized from methanol/DMF. The product had a melting point of 234°-235° C.

후처리

  1. temperatureit was cooled
  2. filtrationThe precipitate was filtered off with suction
  3. customrecrystallized from methanol/DMF

출처 및 근거

ORD 기록
ord-7a905aff7eb147719255a11abbf4dc0b
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849755

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