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Acetyl chloride → HCID 11429511, 화합물

HRID 1808302
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HRID 1808302 반응식
[CH3:1][O:2][CH:3](OC)[C:4]([O:6][CH3:7])=[O:5].C([Cl:13])(=O)C.[C:14]1([P:20]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>II>[Cl-:13].[CH3:1][O:2][CH:3]([P+:20]([C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1)[C:4]([O:6][CH3:7])=[O:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6367Acetyl chlorideHCID 11776TriphenylphosphineHCID 66647Acetic acid, 2,2-dimethoxy-, methyl ester

생성물 1

HCID 11429511HCID 11429511, 화합물수율 93.9%

시약·촉매·용매 1

HCID 807Iodine촉매

반응 조건

온도
55 °C

실험 절차

25 g (0.186 mol) of methyl dimethoxyacetate are added to 27 ml (0.215 mol) of acetyl chloride at ambient temperature. 0.1 g (0.2 mol %) of diiodine are added and then the reaction mixture is stirred at 55° C. for 16 hours. The excess acetyl chloride is evaporated under vacuum and then the residue is dissolved in 100 ml of dichloromethane. 49 g (0.204 mol) of triphenylphosphine are added and then the reaction mixture is stirred at 37° C. for 3 hours. The solvents are evaporated and then the residue is crystallized from diisopropyl ether. 70 g of (methoxy(methoxycarbonyl)methyl)triphenylphosphonium chloride are obtained.

후처리

  1. customThe excess acetyl chloride is evaporated under vacuum
  2. dissolutionthe residue is dissolved in 100 ml of dichloromethane
  3. stirringthe reaction mixture is stirred at 37° C. for 3 hours
  4. customThe solvents are evaporated
  5. customthe residue is crystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-7b9c6ca5a73a4fe9a7d41678b8c86144
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08357819B2

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