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

HRID 65591
ノート
印刷プレビュー

反応式

HRID 65591 の反応式
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:11][CH3:12])([O:9][CH3:10])=[O:8].[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[OH:21])#[N:15]>C(#N)C>[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[O:21][P:7]([O:11][CH3:12])([O:9][CH3:10])=[O:8])#[N:15]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 101863Phosphorochloridic acid, dimethyl esterHCID 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

生成物 1

HCID 213179045-Butoxy-2-cyanothiophen-3-yl dimethyl phosphate収率 76.8%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
20 °C

実験手順

7.7 g of potassium carbonate and 7.7 g of O,O-dimethyl 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 20° C. and was filtered. The filtrate was evaporated to dryness under reduced pressure and the residue was dissolved in ether. The ether solution was washed with water containing 100 g/l of sodium chloride and then with 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride. The ether phase was dried and treated with activated carbon, filtered and concentrated to dryness to obtain 12.5 g of 2-cyano-3-(dimethoxyphosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.511.

後処理

  1. filtrationwas filtered
  2. customThe filtrate was evaporated to dryness under reduced pressure
  3. dissolutionthe residue was dissolved in ether
  4. washThe ether solution was washed with water containing 100 g/l of sodium chloride
  5. additionwith 0.1N sodium hydroxide solution containing 100 g/l of sodium chloride
  6. dry with materialThe ether phase was dried
  7. additiontreated with activated carbon
  8. filtrationfiltered
  9. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-432cda9a55fc428fafdceacba2e3aaea
出典データセット
uspto-grants-1978_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04128562

反応ノート

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