Sodium Carbonate → HCID 57551211, 화합물

HRID 1644649노트

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HRID 1644649 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([NH:12][NH2:13])=O)=[CH:5][CH:4]=1.[N:16]([C:19]1[CH:24]=[CH:23][C:22]([S:25]([NH:28][C:29]2[S:30][CH:31]=[CH:32][N:33]=2)(=[O:27])=[O:26])=[CH:21][CH:20]=1)=[C:17]=[S:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[S:30]1[CH:31]=[CH:32][N:33]=[C:29]1[NH:28][S:25]([C:22]1[CH:21]=[CH:20][C:19]([NH:16][C:17]2[S:18][C:10]([CH2:9][C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:15])([F:14])[F:1])=[CH:4][CH:5]=3)=[N:12][N:13]=2)=[CH:24][CH:23]=1)(=[O:26])=[O:27]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 44674964-isothiocyanato-N-1,3-thiazol-2-ylbenzenesulfonamideHCID 43237029HCID 43237029, 화합물

생성물 1

HCID 57551211HCID 57551211, 화합물수율 20%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
85 °C

실험 절차

A mixture of (4-trifluoromethyl-phenyl)-acetic acid hydrazide (55 mg, 0.25 mmol, 1.5 equiv), 4-isothiocyanato-N-thiazol-2-yl-benzenesulfonamide (50 mg, 0.2 mmol, 1.0 equiv) and sodium carbonate (20 mg, 0.18 mmol, 1.1 equiv) in 1.0 mL of ethanol was heated at 85° C. After 16 h, the heterogeneous reaction mixture was concentrated in vacuo, diluted with 500 μL of acetonitrile, filtered, and purified via reverse phase HPLC. The fraction containing product was lyophilized to afford the product as an off-white solid (15 mg, 20%).

후처리

  1. concentrationthe heterogeneous reaction mixture was concentrated in vacuo
  2. additiondiluted with 500 μL of acetonitrile
  3. filtrationfiltered
  4. custompurified via reverse phase HPLC
  5. additionThe fraction containing product

출처 및 근거

ORD 기록
ord-2fdb93d8572e4a72b3617c5d02932de3
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124610B2

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