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

HRID 65590

反応式

HRID 65590 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 213179365-Butoxy-2-cyanothiophen-3-yl diethyl phosphate収率 93.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e7487320950f418a9e636fd700ecdb7c
出典データセット
uspto-grants-1978_12
特許番号
US04128562

関連ノート

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