Isobutyryl chloride → HCID 59623752、化合物

HRID 1093955ノート

反応式

HRID 1093955 の反応式
C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Cl:13][C:14]1[CH:19]=[C:18]([CH3:20])[CH:17]=[CH:16][C:15]=1[Pb+3].[F:22][CH:23]([F:38])[CH2:24][N:25]1[C:34]2[C:29](=[N:30][CH:31]=[CH:32][N:33]=2)[C:28](=[O:35])[CH2:27][S:26]1(=[O:37])=[O:36].[C:39](Cl)(=[O:43])[CH:40]([CH3:42])[CH3:41]>CN(C)C1C=CN=CC=1.C(Cl)(Cl)Cl.C1(C)C=CC=CC=1.ClCCl.Cl>[Cl:13][C:14]1[CH:19]=[C:18]([CH3:20])[CH:17]=[CH:16][C:15]=1[C:27]1[S:26](=[O:36])(=[O:37])[N:25]([CH2:24][CH:23]([F:22])[F:38])[C:34]2[C:29]([C:28]=1[O:35][C:39](=[O:43])[CH:40]([CH3:42])[CH3:41])=[N:30][CH:31]=[CH:32][N:33]=2

参加物

9

反応物 3

HCID 62325Isobutyryl chlorideHCID 59623757HCID 59623757、化合物HCID 178476527HCID 178476527、化合物

生成物 1

HCID 59623752HCID 59623752、化合物

試薬・触媒・溶媒 5

HCID 142844-(Dimethylamino)pyridine触媒HCID 313Hydrochloric Acid溶媒HCID 1140Toluene溶媒HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 2-chloro-4-methyl-phenyl lead triacetate (0.153 g), 1-(2,2-difluoro-ethyl)-2,2-dioxo-2,3-dihydro-1H-2-λ-6-thia-1,5,8-triaza-naphthalen-4-one (Example 9.4) (0.070 g) and 4-dimethylaminopyridine (“DMAP”) (0.169 g) in anhydrous chloroform (2 ml) and toluene (1 ml) under a nitrogen atmosphere was heated to reflux for four hours. Isobutyryl chloride (53 μl) was added and the reaction mixture heated to reflux for a further two hours. The reaction mixture was then allowed to cool to ambient temperature and diluted with dichloromethane and aqueous hydrochloric acid (2M). The solids were removed by filtration and the filtrate was separated. The aqueous layer was extracted with further dichloromethane. The combined organic extracts were concentrated. The residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane 1:6) to give Compound No. C136 of Table C (0.019 g).

後処理

  1. temperaturewas heated
  2. temperatureto reflux for four hours
  3. temperaturethe reaction mixture heated
  4. temperatureto reflux for a further two hours
  5. customThe solids were removed by filtration
  6. customthe filtrate was separated
  7. extractionThe aqueous layer was extracted with further dichloromethane
  8. concentrationThe combined organic extracts were concentrated
  9. customThe residue was purified by column chromatography on silica gel (eluent: ethyl acetate/hexane 1:6)
  10. customto give Compound No

出典と根拠

ORDレコード
ord-47bc5fc963164db8a1f226c8b5517b39
出典データセット
uspto-grants-2012_03
特許番号
US08133849B2

反応ノート

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