Sodium Carbonate → HCID 59464778, 화합물

HRID 1714588

반응식

HRID 1714588 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([S:15][C:16]2[CH:23]=[CH:22][C:19]([CH:20]=O)=[C:18]([Cl:24])[CH:17]=2)[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(OP([CH2:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])(OCC)=O)C.C(=O)(O)[O-].[K+].C(=O)(O)[O-].[Na+].C(=O)([O-])[O-].[K+].[K+].C(=O)([O-])[O-].[Na+].[Na+]>O.CS(C)=O.CN(C)C=O>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([S:15][C:16]2[CH:23]=[CH:22][C:19]([CH:20]=[CH:33][C:34]([O:36][CH2:37][CH3:38])=[O:35])=[C:18]([Cl:24])[CH:17]=2)[CH:12]=[CH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

10

반응물 6

HCID 10340Sodium CarbonateHCID 11430Potassium CarbonateHCID 13345Triethyl phosphonoacetateHCID 516892Sodium BicarbonateHCID 516893Potassium BicarbonateHCID 166554054-(3-Benzyloxyphenylthio)-2-chlorobenzaldehyde

생성물 1

HCID 59464778HCID 59464778, 화합물

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A mixture of 4-(3-benzyloxyphenylthio)-2-chlorobenzaldehyde (1) and ethyl diethylphosphonoacetate (2) is stirred for 3 to 8 hours at 50 to 80° C. in an organic solvent, such as dimethylformamide or dimethylsulfoxide, in the presence of a base, such as potassium bicarbonate, sodium bicarbonate, potassium carbonate or sodium carbonate. Subsequently, the reaction mixture is chilled in an ice water bath while being stirred and water is added. The resulting crystals are collected by filtration and washed with aqueous 2-propanol to give ethyl 3-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]acrylate (3) as crude crystals. This product is dissolved in ethylacetate and the mixture was washed with water. The organic layer is concentrated under reduced pressure to obtain a pale yellow oil. To this product, acetone is added and the mixture is stirred while being chilled to form crystals (Crystal seeds are added when necessary). Water is then added and the mixture is stirred while being chilled. The resulting crystals are collected by filtration and washed with acetone-water. The crystals are then dried at 40° C. or below to give ethyl 3-[4-(3-benzyloxyphenylthio)-2-chlorophenyl]acrylate (3) or a hydrate thereof.

후처리

  1. temperatureSubsequently, the reaction mixture is chilled in an ice water bath
  2. filtrationThe resulting crystals are collected by filtration
  3. washwashed with aqueous 2-propanol

출처 및 근거

ORD 기록
ord-4a062d7335ec45b58e606242b48284ca
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07795472B2

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