Diisopropylethylamine → HCID 58930368, 화합물

HRID 852432노트

반응식

HRID 852432 반응식
CN([CH:4]=[N:5][C:6]([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([S:15]([CH3:18])(=[O:17])=[O:16])[CH:10]=1)=[S:7])C.[F:19][C:20]1[CH:29]=[CH:28][CH:27]=[CH:26][C:21]=1[C:22](=[O:25])[CH2:23]Br.C(N(C(C)C)CC)(C)C>CN(C=O)C>[F:19][C:20]1[CH:29]=[CH:28][CH:27]=[CH:26][C:21]=1[C:22]([C:23]1[S:7][C:6]([NH:8][C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([S:15]([CH3:18])(=[O:16])=[O:17])[CH:10]=2)=[N:5][CH:4]=1)=[O:25]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 27374492-Bromo-2'-fluoroacetophenoneHCID 724664321-Dimethylaminomethylene-3-(3-methanesulfonyl-phenyl)-thiourea

생성물 1

HCID 58930368HCID 58930368, 화합물수율 79%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 37 mg (0.13 mmol) 1-Dimethylaminomethylene-3-(3-methanesulfonyl-phenyl)-thiourea in 0.33 ml DMF was added 28 mg (0.13 mmol) 2-Fluorophenacyl bromide and the mixture was allowed to stir at room temperature for 16 h. 17 mg (0.13 mmol) diisopropylethylamine was added and the mixture was subjected to preparative HPLC separation on reversed phase eluting with an acetonitrile/water gradient to yield 38.5 mg (79%) of the title compound after evaporation of the product fractions.

후처리

  1. customHPLC separation on reversed phase
  2. washeluting with an acetonitrile/water gradient

출처 및 근거

ORD 기록
ord-fdb8a297940f4ff0b53f4ac12f606c42
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07253197B2

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