Hydrochloric Acid → HCID 53662138, 화합물

HRID 1680275

반응식

HRID 1680275 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[CH3:5][O:6][C:7]([CH:9]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11][CH2:10]1)=[O:8].[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.Cl>C(=S)=S>[CH3:5][O:6][C:7]([CH:9]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([C:18](=[O:25])[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH:16]=2)[CH2:11][CH2:10]1)=[O:8]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 3839612Methyl 2,3-dihydro-1H-indene-1-carboxylateHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 53662138HCID 53662138, 화합물

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

18 g of finely powdered aluminium chloride are added in portions to a solution of 8 g of indane-1-carboxylic acid methyl ester and 8.2 g of benzoyl chloride in 100 ml of carbon disulphide, whilst stirring in an anhydrous atmosphere. After completion of the addition, the reaction mixture is heated for 2 hours to the reflux temperature. It is then allowed to cool to room temperature, poured onto a mixture of 100 g of ice and 50 ml of concentrated hydrochloric acid and extracted with twice 100 ml of ether. The organic phases are combined, washed with twice 100 ml of water, dried over sodium sulphate and evaporated in vacuo. Distillation of the evaporation residue in a high vacuum gives 6-benzoyl-indane-1-carboxylic acid methyl ester in the fraction boiling at 165°-170° C. (0.5 mm).

후처리

  1. additionAfter completion of the addition
  2. temperaturethe reaction mixture is heated for 2 hours to the reflux temperature
  3. extractionextracted with twice 100 ml of ether
  4. washwashed with twice 100 ml of water
  5. dry with materialdried over sodium sulphate
  6. customevaporated in vacuo
  7. distillationDistillation of the evaporation residue in a high vacuum

출처 및 근거

ORD 기록
ord-0d172210c6e8439a992531a2881941e9
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04272547

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