Iodine → Tris(2-methoxyethoxymethyl)phosphine

HRID 1195633

반응식

HRID 1195633 반응식
II.[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8]Cl.[C:10](=[O:12])=O.C[C:14](C)=[O:15].[Cl-].[CH2:18]1[CH2:22][O:21][CH2:20]C1.[P:23](Cl)(Cl)Cl.[CH2:27]1[CH2:31][O:30][CH2:29]C1>[Hg](Br)Br>[CH3:3][O:4][CH2:5][CH2:6][O:7][CH2:8][P:23]([CH2:20][O:21][CH2:22][CH2:18][O:12][CH3:10])[CH2:14][O:15][CH2:27][CH2:31][O:30][CH3:29]

참가 물질

8

반응물 6

HCID 807IodineHCID 8028TetrahydrofuranHCID 24387Phosphorus trichlorideHCID 775901-(Chloromethoxy)-2-methoxyethaneHCID 18522661Acetone cardiceHCID 21908598chloride THF

생성물 1

HCID 54193331Tris(2-methoxyethoxymethyl)phosphine

시약·촉매·용매 1

HCID 24612Mercury dibromide촉매

반응 조건

온도
-78 °C

실험 절차

To ground Mg metal (5.2 g, 214 mmol) was added I2 (1 crystal), HgBr2 (10 mg) and 2 ml of a solution of 2-methoxyethoxymethyl chloride (25 g, 201 mmol) in THF (100 ml) at R.T. After 30 sec, the reaction started and was cooled to -30° C. (dry-ice/acetone). The remaining chloride/THF solution was added dropwise at -20° to -10° C. over 2 h. The mixture was stirred at 0° C. for 2h post-addition and cooled to -78° C. The reagent was then treated with PCl3 (2.2 ml, 25.1 mmol) according to General Method I and the final residue was purified by distillation to afford 1.6 (21%) of tris(2-methoxyethoxymethyl)phosphine as a colorless mobile oil (b.p.=150°-160° [email protected] mmHg). 31P-NMR(CDCl3): -42.7. MS(LREI)m/z=299(M+1 ).

후처리

  1. distillationthe final residue was purified by distillation

출처 및 근거

ORD 기록
ord-a608e555ca3c45e790ed0ca057610d93
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112595

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