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Acetyl chloride → HCID 11429511, 화합물

HRID 1951975
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반응식

HRID 1951975 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 (186 mmol) of methyl dimethoxyacetate is added to 27 ml (215 mmol) of acetyl chloride at room temperature. 0.1 g (0.2% molar) of iodine is added and then the reaction mixture is stirred at 55° C. for 16 hours. The excess of acetyl chloride is evaporated under vacuum, then the residue is dissolved in 100 ml of dichloromethane. 49 g (204 mmol) of triphenylphosphine is added and then the reaction mixture is stirred at 37° C. for 3 hours. The solvents are evaporated and the residue is crystallized in diisopropyl ether. 70 g (88%) of (methoxy-methoxycarbonyl-methyl)-triphenyl-phosphonium chloride is obtained.

후처리

  1. customThe excess of 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 in diisopropyl ether

출처 및 근거

ORD 기록
ord-60f60fc882b64f879e47448bf4b856fe
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404836B2

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