Diazomethane → HCID 13076873, 화합물

HRID 1438727노트

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HRID 1438727 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][C@H:7]([C:16]([OH:18])=[O:17])[O:8][C@H:9]([C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:4]=2[CH:3]=1.[N+](=[CH2:23])=[N-]>CCOCC>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]2[O:6][C@H:7]([C:16]([O:18][CH3:23])=[O:17])[O:8][C@H:9]([C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 9550Diazomethane2회HCID 12812406HCID 12812406, 화합물

생성물 1

HCID 13076873HCID 13076873, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To an ether solution of cis-6-chloro-4-phenyl-1,3-benzodioxan-2-carboxylic acid (2.14 g, 7.36 mmoles), chilled in an ice bath, was added an ethereal solution of diazomethane until the yellow color of the diazomethane was no longer discharged. The solution was stirred in the ice bath for 10 minutes at room temp. for 10 minutes, and finally at 35° for 15 minutes. The ether solution was washed with dil.NaHCO3 solution (2 portions), water (2 portions), and saturated brine (1 portion), and dried over anhydrous Na2SO4. The solvent was evaporated to yield a solid which was recrystallized from benzene-Skellysolve B (essentially n-hexane). The yield was 1.71 g (76%); m.p. 129.5°-131°. NMR (CDCl3), β6.6 (d, 1H, C(5)H, cis); 5.65 ppm (s, 1H, C(2)H, cis).

후처리

  1. washThe ether solution was washed with dil
  2. dry with materialNaHCO3 solution (2 portions), water (2 portions), and saturated brine (1 portion), and dried over anhydrous Na2SO4
  3. customThe solvent was evaporated
  4. customto yield a solid which
  5. customwas recrystallized from benzene-Skellysolve B (essentially n-hexane)

출처 및 근거

ORD 기록
ord-029b35d05f16401695956a36d38207da
출처 데이터셋
uspto-grants-1977_11
특허 번호
US04056540

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