Diphenyl Ether → 3-(8-Chloro-dibenz[b,f][1,4]oxazepin-10(11H)-yl)-4-ethoxy-3-cyclobutene-1,2-dione

HRID 1707577

반응식

HRID 1707577 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH:9]=[N:10][C:4]=2[CH:3]=1.[CH2:17]([O:19][C:20]1[C:21](=O)[C:22](=[O:27])[C:23]=1[O:24]CC)[CH3:18].C1(OC2C=CC=CC=2)C=CC=CC=1>O1CCOCC1>[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9][N:10]([C:21]3[C:22](=[O:27])[C:23](=[O:24])[C:20]=3[O:19][CH2:17][CH3:18])[C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 7583Diphenyl EtherHCID 123228Diethyl squarateHCID 8382678-Chloro-dibenz[b,f]-[1,4]oxazepine

생성물 1

HCID 152322933-(8-Chloro-dibenz[b,f][1,4]oxazepin-10(11H)-yl)-4-ethoxy-3-cyclobutene-1,2-dione

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 8-chloro-dibenz[b,f][1,4]oxazepine (2 g), 3,4-diethoxy-3-cyclobutene-1,2-dione (5 g), diphenylether (2 g) and dioxane (10 mL) was heated to reflux. After 2 hours, most of the dioxane was removed in vacuo and the precipitated title compound (0.75 g) was collected by filtration as yellow solid. The filtrate was treated with cold methanol when more of the title compound (1.2 g) precipitated. This material was used in Example 6 without further purification.

후처리

  1. temperaturewas heated to reflux
  2. custommost of the dioxane was removed in vacuo
  3. customthe precipitated title compound (0.75 g)
  4. filtrationwas collected by filtration as yellow solid
  5. additionThe filtrate was treated with cold methanol when more of the title compound (1.2 g)
  6. customprecipitated
  7. customThis material was used in Example 6 without further purification

출처 및 근거

ORD 기록
ord-57f9b35e48a04aa2872b5c7c2667e77f
출처 데이터셋
uspto-grants-1994_10
특허 번호
US05354746

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