1-Propanol → HCID 12521033, 화합물

HRID 1857341

반응식

HRID 1857341 반응식
[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]

참가 물질

5

반응물 3

HCID 10311-PropanolHCID 73907Phosphorodichloridothioic acid, O-ethyl esterHCID 236693631-Propanol, sodium salt (1:1)

생성물 1

HCID 12521033HCID 12521033, 화합물수율 59.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-deff895b5cbf47998e8bbee8d1ac0ed1
출처 데이터셋
uspto-grants-2000_11
특허 번호
US06147062

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