1-Propanol → HCID 12521033、化合物

HRID 1857341

反応式

HRID 1857341 の反応式
[P:1](Cl)([Cl:6])([O:3][CH2:4][CH3:5])=[S:2].[O-:8][CH2:9][CH2:10][CH3:11].[Na+].C(O)CC>O1CCCC1>[P:1]([Cl:6])([O:8][CH2:9][CH2:10][CH3:11])([O:3][CH2:4][CH3:5])=[S:2]

参加物

5

反応物 3

HCID 10311-PropanolHCID 73907Phosphorodichloridothioic acid, O-ethyl esterHCID 236693631-Propanol, sodium salt

生成物 1

HCID 12521033HCID 12521033、化合物収率 59.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To 30 g (167 mmole) of O-ethyl dichlorothiophosphate in 100 ml of tetrahydrofuran (THF) cooled to -70° C. was added a solution of sodium propoxide (from 7.4 g of 60% NaH (184 mmole) and 11 g (176 mmole) of 1-propanol) in 50 ml of THF. After warming to room temperature over 2 hours, the THF was removed in vacuo and the residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water. The organic layer was dried over magnesium sulfate, concentrated in vacuo, and distilled (bp 45-50° C. 1 torr) yielding 20 g of the title compound, an oil. nmr 1.0 t 3H, 1.4 t 3H, 1.8 sextet 2H, 4.4 m 4H.

後処理

  1. customthe THF was removed in vacuo
  2. customthe residue was partitioned between 50 ml diethyl ether, 50 ml hexanes, and 25 ml cold water
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. distillationdistilled (bp 45-50° C. 1 torr)

出典と根拠

ORDレコード
ord-deff895b5cbf47998e8bbee8d1ac0ed1
出典データセット
uspto-grants-2000_11
特許番号
US06147062

関連ノート

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