Dichloromethane → HCID 22397175, 화합물

HRID 411222노트

반응식

HRID 411222 반응식
BrN1C(=O)CCC1=O.[CH3:9][N:10]1[C:15]2[CH:16]=[CH:17][C:18]([CH3:20])=[CH:19][C:14]=2[S:13](=[O:22])(=[O:21])[C:12]([C:23]([O:25][CH3:26])=[O:24])=[N:11]1.[NH:27]1[CH2:32][CH2:31][O:30][CH2:29][CH2:28]1.C(Cl)Cl>ClC(Cl)C.CN(C=O)C>[CH3:9][N:10]1[C:15]2[CH:16]=[CH:17][C:18]([CH2:20][N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)=[CH:19][C:14]=2[S:13](=[O:22])(=[O:21])[C:12]([C:23]([O:25][CH3:26])=[O:24])=[N:11]1

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 8083MorpholineHCID 67184N-bromobutanimideHCID 22397147HCID 22397147, 화합물

생성물 1

HCID 22397175HCID 22397175, 화합물수율 59%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 63651,1-Dichloroethane용매

실험 절차

N-Bromosuccinimide (0.239 g) and methyl 1,6-dimethyl-1H-4,1,2-benzothiadiazine-3-carboxylate 4,4-dioxide (Preparation 40, 0.30 g) are dissolved in dichloroethane (100 mL). The solution is exposed to light from a 650 W sunlamp with stirring for 25 minutes. The solvent is evaporated and the crude solid obtained is dissolved in DMF (8 mL). Morpholine (0.43 g) is added and the mixture is stirred for 3 hours. The mixture is poured into CH2Cl2 (200 mL) and washed with water (3×200mL). The organic layer is dried with Na2SO4, filtered and the solvent evaporated. The crude solid is chromatographed with MeOH/CH2Cl2 (1-5%) to obtain 0.23 g (59%) of the title compound as an off-white solid. Physical characteristics: MS (ESI+) m/z 254 (M+H).

후처리

  1. customThe solvent is evaporated
  2. customthe crude solid obtained
  3. stirringthe mixture is stirred for 3 hours
  4. washwashed with water (3×200mL)
  5. dry with materialThe organic layer is dried with Na2SO4
  6. filtrationfiltered
  7. customthe solvent evaporated
  8. customThe crude solid is chromatographed with MeOH/CH2Cl2 (1-5%)

출처 및 근거

ORD 기록
ord-b66b46c3fccf40bc961f3a6a3e2248f9
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559145B2

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