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Acetone → HCID 131719649, 화합물

HRID 1900879
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인쇄 미리보기

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HRID 1900879 반응식
[C:1]([C:4]1[N:9]=[CH:8][C:7]([C:10]([NH:12][C:13](=[O:30])[NH:14][C:15]2[CH:29]=[CH:28][C:18]([O:19][CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])=[CH:17][CH:16]=2)=[O:11])=[CH:6][CH:5]=1)(=S)[NH2:2].IC.CC(C)=O.C([O-])(=O)C.[NH4+:41]>ClCCl.CO>[C:21]([OH:23])(=[O:22])[CH3:20].[C:1]([C:4]1[N:9]=[CH:8][C:7]([C:10]([NH:12][C:13](=[O:30])[NH:14][C:15]2[CH:29]=[CH:28][C:18]([O:19][CH2:20][C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])=[CH:17][CH:16]=2)=[O:11])=[CH:6][CH:5]=1)(=[NH:41])[NH2:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 517165Ammonium AcetateHCID 23370042HCID 23370042, 화합물

생성물 1

HCID 131719649HCID 131719649, 화합물수율 111.9%

시약·촉매·용매 2

HCID 887Methanol용매
HCID 6344
Dichloromethane
용매

실험 절차

In a similar manner to Example 1, t-butyl 4-[3-(6-thiocarbamoylpyrid-3-ylcarbonyl)ureido]phenoxyacetate (2.73 g) was reacted with iodomethane (13 ml) and acetone (200 ml) and the resultant product was treated with ammonium acetate (6 g), methanol (30 ml) and dichloromethane (30 ml) at ambient temperature. This yielded a crude solid which was collected and washed with methanol and acetone to give the title compound (1.68 g) as an orange solid: m.p. 290°-300° C. (decomposes); NMR Spectrum (DMSO-d6) 1.43 (9H, s), 1.82 (3H, s), 4.62 (2H, s), 6.90 (2H, d), 7.49 (2H, d), 8.29 (1H, d), 8.52 (1H, dd), 9.18 (1H, d) 10.61 (1H, s); Mass Spectrum m/Z 414 (M+H)+ ; Elemental Analysis: calculated for C20H23N5O5. 1.0 CH3CO2H. 0.5 H2O: C, 54.8%; H, 5.85%; N, 14.5%; found: C, 54.6%; H, 6.0%; N, 14.5%

후처리

  1. customThis yielded a crude solid which
  2. customwas collected
  3. washwashed with methanol and acetone

출처 및 근거

ORD 기록
ord-c5875644858e4741b13f454250fd5242
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05576334

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