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Lawesson's reagent → HCID 11305607, 화합물

HRID 1271072
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HRID 1271072 반응식
COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:10]2)=CC=1.[Cl:23][C:24]1[CH:54]=[CH:53][C:27]([CH2:28][N:29]2[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:31]([C:38](=O)[C:39]([NH:41][C:42]3[CH:43]=[C:44]4[C:49](=[CH:50][CH:51]=3)[N:48]=[CH:47][CH:46]=[CH:45]4)=[O:40])=[CH:30]2)=[CH:26][CH:25]=1>C1(C)C=CC=CC=1>[Cl:23][C:24]1[CH:54]=[CH:53][C:27]([CH2:28][N:29]2[C:37]3[C:32](=[CH:33][CH:34]=[CH:35][CH:36]=3)[C:31]([C:38](=[S:10])[C:39]([NH:41][C:42]3[CH:43]=[C:44]4[C:49](=[CH:50][CH:51]=3)[N:48]=[CH:47][CH:46]=[CH:45]4)=[O:40])=[CH:30]2)=[CH:26][CH:25]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 10203597Entasobulin

생성물 1

HCID 11305607HCID 11305607, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
75 °C

실험 절차

3.68 g (9.1 mMol) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide are added, under nitrogen, to a suspension of 4.00 g (9.1 mMol) of 2-[1-(4-chlorobenzyl)-1H-indol-3-yl]-2-oxo-N-quinolin-6-ylacetamide in 200 ml of toluene, after which the mixture is heated at 75° C. for 3 h. The residue which has formed is filtered off in the hot from the reaction solution and subsequently washed with 100 ml of methylene chloride. The filtrate is concentrated in vacuo and the residue is chromatographed on flash silica gel (eluent: methylene chloride/methanol 99:1). The product fractions are filtered on flash silica gel (eluent: n-heptane/ethyl acetate 1:1) after the solvent has been removed once more.

후처리

  1. customThe residue which has formed
  2. filtrationis filtered off in the hot from the reaction solution
  3. washsubsequently washed with 100 ml of methylene chloride
  4. concentrationThe filtrate is concentrated in vacuo
  5. customthe residue is chromatographed on flash silica gel (eluent: methylene chloride/methanol 99:1)
  6. filtrationThe product fractions are filtered on flash silica gel (eluent: n-heptane/ethyl acetate 1:1) after the solvent
  7. customhas been removed once more

출처 및 근거

ORD 기록
ord-1335eade7bc24499b9a2e5f1e4a479d7
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07205299B2

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