Triethylamine → HCID 57269752、化合物

HRID 1632217ノート

反応式

HRID 1632217 の反応式
[Cl:1][C:2]1[C:15]2[C:6](=[CH:7][C:8]3[C:13]([CH:14]=2)=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:5]=[C:4]([OH:16])[CH:3]=1.C(N(CC)CC)C.[P:24](=[O:32])(Cl)([S:27][CH2:28][CH2:29][CH3:30])[O:25][CH3:26].C(OCC)(=O)C>C1(C)C=CC=CC=1>[P:24](=[O:32])([S:27][CH2:28][CH2:29][CH3:30])([O:16][C:4]1[CH:3]=[C:2]([Cl:1])[C:15]2[C:6](=[CH:7][C:8]3[C:13]([CH:14]=2)=[CH:12][CH:11]=[CH:10][CH:9]=3)[CH:5]=1)[O:25][CH3:26]

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 12917781Phosphorochloridothioic acid, O-methyl S-propyl esterHCID 20443614HCID 20443614、化合物

生成物 1

HCID 57269752HCID 57269752、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

4-Chloro-2-anthrol (0.01 mole), triethylamine (0.01 mole) tetrahydrofuran (25 ml) and toluene (25 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer and thermometer. The mixture is cooled to a temperature of about 0° C. and O-methyl S-propyl phosphorochloridothioate (0.01 mole) dissolved in toluene (25 ml) is added with stirring over a period of about 30 minutes. After the addition is completed the reaction mixture is allowed to warm to room temperature and stirring is continued for a period of about 16 hours. After this time the reaction mixture is filtered to remove triethylamine hydrochloride. The filtrate is then washed with water, dried over anhydrous magnesium sulfate and stripped of solvents leaving a residue. This residue is subjected to flash chromatography using ethyl acetate as the eluant to yield the desired product O-methyl O-(4-chloro-2-anthryl) S-propyl phosphorothioate.

後処理

  1. customequipped with a mechanical stirrer
  2. additionis added
  3. additionAfter the addition
  4. stirringstirring
  5. waitis continued for a period of about 16 hours
  6. filtrationAfter this time the reaction mixture is filtered
  7. customto remove triethylamine hydrochloride
  8. washThe filtrate is then washed with water
  9. dry with materialdried over anhydrous magnesium sulfate
  10. customleaving a residue

出典と根拠

ORDレコード
ord-e7b33939738a480ca4835e7315b39ad0
出典データセット
uspto-grants-1984_10
特許番号
US04474776

反応ノート

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