Dichloromethane → HCID 11417330、化合物

HRID 896845ノート

反応式

HRID 896845 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([CH3:12])[C:3]=1[C:4]([OH:6])=O.ClCCl.[CH3:16][O:17][C:18]1[CH:19]=[C:20]([CH3:28])[CH:21]=[C:22]([O:26][CH3:27])[C:23]=1[O:24][CH3:25].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C(OC)(C)(C)C.CCCCCC.O>[Cl:1][C:2]1[CH:10]=[CH:9][C:8]([Cl:11])=[C:7]([CH3:12])[C:3]=1[C:4]([C:21]1[C:22]([O:26][CH3:27])=[C:23]([O:24][CH3:25])[C:18]([O:17][CH3:16])=[CH:19][C:20]=1[CH3:28])=[O:6]

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 14812Phosphorus oxide (P4O10)HCID 809223,4,5-TrimethoxytolueneHCID 111950733,6-Dichloro-2-methylbenzoic acid

生成物 1

HCID 11417330HCID 11417330、化合物収率 88.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21982663Methyl t-butylether hexane溶媒

実験手順

14 g (68.29 mmol) of 2,5-dichloro-6-methylbenzoic acid were introduced into 1000 ml of dichloromethane. 11.2 g (61.6 mmol) of 3,4,5-trimethoxytoluene and 28 g of finely ground phosphorus pentoxide were added. After 2 hours of stirring at room temperature, the reaction solution, which by now was orangey red, was poured into water and extracted three times with dichloromethane. The combined organic phases were washed twice with water, dried with sodium sulfate and concentrated, and the reaction product was then isolated by column chromatography using a methyl tert-butyl ether/hexane gradient. This gave 20.1 g of the title compound (yield 80%).

後処理

  1. extractionextracted three times with dichloromethane
  2. washThe combined organic phases were washed twice with water
  3. dry with materialdried with sodium sulfate
  4. concentrationconcentrated
  5. customthe reaction product was then isolated by column chromatography

出典と根拠

ORDレコード
ord-ea9a12b0c1e54f7fb59341ba4c6d11ac
出典データセット
uspto-grants-2005_07
特許番号
US06919485B2

反応ノート

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