Dichloromethane → HCID 11417330, 화합물

HRID 896845노트

반응식

HRID 896845 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 11417330HCID 11417330, 화합물수율 88.4%

시약·촉매·용매 2

HCID 962Water용매HCID 21982663Methyl t-butylether hexane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-ea9a12b0c1e54f7fb59341ba4c6d11ac
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919485B2

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