Potassium Carbonate → 5-Butoxy-2-cyanothiophen-3-yl diethyl phosphate

HRID 65590

반응식

HRID 65590 반응식
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[O:8].[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[OH:23])#[N:17]>C(#N)C>[C:16]([C:18]1[S:19][C:20]([O:24][CH2:25][CH2:26][CH2:27][CH3:28])=[CH:21][C:22]=1[O:23][P:7]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[O:8])#[N:17]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 13139Diethyl chlorophosphateHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

생성물 1

HCID 213179365-Butoxy-2-cyanothiophen-3-yl diethyl phosphate수율 93.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

7.7 g of potassium carbonate and 8.6 g of O,O-diethyl chlorophosphate were added to a solution of 11 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 16 hours at room temperature and was then filtered. The filtrate was evaporated to dryness and the residue was taken up in ethyl ether. The ether phase was washed with an aqueous solution of 100 g/l of sodium chloride and then with an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The solution was dried, treated with activated carbon, filtered and evaporated to dryness under reduced pressure to obtain 15.5 g of 2-cyano-3-(diethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.500.

후처리

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. washThe ether phase was washed with an aqueous solution of 100 g/l of sodium chloride
  4. additionwith an aqueous 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride
  5. customThe solution was dried
  6. additiontreated with activated carbon
  7. filtrationfiltered
  8. customevaporated to dryness under reduced pressure

출처 및 근거

ORD 기록
ord-e7487320950f418a9e636fd700ecdb7c
출처 데이터셋
uspto-grants-1978_12
특허 번호
US04128562

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