반응 #1929096

반응 방정식

Sulfuryl chloride

61

S-Ethyl O-(4,4-bis(diethylphosphono)butanoyloxy)methyl carbonothioate

→

(Carbonochloridoyloxy)methyl 4,4-bis(diethylphosphono)butanoate

반응 조건

후처리

1. 1
   기타The neat reaction
2. 2
   기타The excess sulfuryl chloride was removed under reduced pressure
3. 3
   기타resulting in chloroformate 62 (1.87 g, 97%) that
4. 4
   기타was used without purification

실험 절차

Sulfuryl chloride (687 μL, 8.49 mmol) was added drop-wise to 61 (2.03 g, 4.24 mmol). The neat reaction was stirred at room temperature for 2.5 hr. The excess sulfuryl chloride was removed under reduced pressure resulting in chloroformate 62 (1.87 g, 97%) that was used without purification. 1H NMR (400 MHz, CDCl3): δ 1.35 (t, J=7.1, 12H), 2.17-2.36 (m, 2H), 2.53 (tt, J=23.8, 6.5, 1H), 2.80 (t, J=7.5, 2H), 4.15-4.24 (m, 8H), 5.82 (s, 2H). 31P NMR (162 MHz, CDCl3) δ 23.72 (s, 2P).

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