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Lawesson's reagent → HCID 11305607、化合物

HRID 1271072
ノート
印刷プレビュー

反応式

HRID 1271072 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 10203597Entasobulin

生成物 1

HCID 11305607HCID 11305607、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
75 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1335eade7bc24499b9a2e5f1e4a479d7
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07205299B2

反応ノート

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