반응 #62057

반응 방정식

NaHCO3

1

4-Chloro-4-(2,2,2-trichloro-ethyl)-oxetan-2-one

morpholine

→

2

5,5-Dichloro-1-morpholin-4-yl-pent-4-ene-1,3-dione

용매

DCM

DCM

TBME

반응 조건

후처리

1. 1
   여과The reaction was filtered
2. 2
   세척washed with DCM (3×100 ml)
3. 3
   농축the combined organic layers were concentrated in vacuo to a slurry which
4. 4
   세척further washed with DCM (4×100 ml)
5. 5
   농축The combined organic layers were concentrated in vacuo
6. 6
   workup.STIRRINGstirred for 1 hour
7. 7
   여과filtered
8. 8
   기타dried
9. 9
   기타to give a cream solid
10. 10
    workup.STIRRINGstirred for 15 minutes
11. 11
    여과filtered
12. 12
    세척washed with TBME
13. 13
    기타dried

실험 절차

Two separate solutions of 1 (62.5 g, 0.26 mmol) and morpholine (24.0 g, 0.28 mol) in DCM (120 ml) were added simultaneously to a mixture of NaHCO3 (44.0 g, 0.52 mol) in dry DCM (300 ml). The reaction was maintained at 15° C. over 140 minutes with stirring. The reaction was filtered, washed with DCM (3×100 ml) and the combined organic layers were concentrated in vacuo to a slurry which was then passed through a short silica pad, and further washed with DCM (4×100 ml). The combined organic layers were concentrated in vacuo, suspended in hexane (400 ml) and stirred for 1 hour, filtered and dried to give a cream solid. The solid was suspended in TBME (100 ml), stirred for 15 minutes, filtered, washed with TBME and dried to give 2 as a white powder (47.8 g, 72%). m/z (LC-MS, ESP): 252 (M++1).

출처