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Sodium Chloride → HCID 53934759、化合物

HRID 444304
ノート
印刷プレビュー

反応式

HRID 444304 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:17]=[CH:16][CH:15]=[CH:14][C:5]=1[CH:6]=[CH:7][C:8]1[S:9][C:10]([CH3:13])=[N:11][N:12]=1.[Cl-].[Na+].[O:20]1[CH2:24]C[CH2:22][CH2:21]1>CN(P(N(C)C)(N(C)C)=O)C>[CH3:13][C:10]1[S:9][C:8]([CH:7]=[CH:6][C:5]2[CH:14]=[CH:15][CH:16]=[CH:17][C:4]=2[O:3][CH2:22][CH:21]2[O:20][CH2:24]2)=[N:12][N:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 136139912HCID 136139912、化合物

生成物 1

HCID 53934759HCID 53934759、化合物

試薬・触媒・溶媒 1

HCID 12679Hexamethylphosphoramide溶媒

実験手順

3.72 g (0.085 mole) of 55% strength sodium hydride in paraffin oil are suspended in 150 ml of absolute tetrahydrofuran and 18.6 g (0.085 mole) of 2-(2-hydroxystyryl)-5-methyl-1,3,4-thiadiazole in 200 ml of absolute hexamethylphosphotriamide are then added dropwise in the course of 1.5 hours at from 0° to 3° C. Stirring is continued at room temperature for 1 hour, after which 11.7 g (0.085 mole) of dibromohydrin are added dropwise. The solution is left to stand at room temperature for 16 hours, after which it is poured onto 1.5 liters of ice water and 0.5 liter of saturated sodium chloride solution. The precipitated solid is filtered off and recrystallized from acetone. 11.8 g (51% of theory) of yellow crystals, of melting point 134°-135° C. are obtained.

後処理

  1. additionafter which 11.7 g (0.085 mole) of dibromohydrin are added dropwise
  2. waitThe solution is left
  3. waitto stand at room temperature for 16 hours
  4. filtrationThe precipitated solid is filtered off
  5. customrecrystallized from acetone
  6. custom11.8 g (51% of theory) of yellow crystals, of melting point 134°-135° C. are obtained

出典と根拠

ORDレコード
ord-6a247671397c4959b8dcda95fda621f5
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04263430

反応ノート

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