Toluene → 8-chlorodibenz[b,f][1,4]oxazepin-10(11H)carbonyl chloride

HRID 128644

반응식

HRID 128644 반응식
[C:1]([Cl:4])(Cl)=[O:2].C1(C)C=CC=CC=1.[Cl:12][C:13]1[CH:27]=[CH:26][C:16]2[O:17][C:18]3[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=3[CH2:20][NH:21][C:15]=2[CH:14]=1>CCOCC.C(N(CC)CC)C>[Cl:12][C:13]1[CH:27]=[CH:26][C:16]2[O:17][C:18]3[CH:25]=[CH:24][CH:23]=[CH:22][C:19]=3[CH2:20][N:21]([C:1]([Cl:4])=[O:2])[C:15]=2[CH:14]=1

참가 물질

6

반응물 3

HCID 1140TolueneHCID 6371PhosgeneHCID 152292278-Chloro-10,11-dihydrodibenzo[b,f][1,4]oxazepine

생성물 1

HCID 149759838-chlorodibenz[b,f][1,4]oxazepin-10(11H)carbonyl chloride

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8471Triethylamine용매

실험 절차

13 parts of phosgene in 45 parts of toluene was stirred for 2 hours at 5°-10° C., and then 70 parts of ether was added. This was followed by the addition of a solution of 18.9 parts of 8-chloro-10,11-dihydrodibenz[b,f][1,4]oxazepine and 7.2 parts of triethylamine in 140 parts of ether. After the addition was complete, the mixture was stirred for 2 hours, and then was filtered. The solvent was then evaporated from the filtrate. The resulting residue was then dissolved in 200 parts by volume of hot hexane, and this mixture was then filtered and cooled.

후처리

  1. additionAfter the addition
  2. filtrationwas filtered
  3. customThe solvent was then evaporated from the filtrate
  4. dissolutionThe resulting residue was then dissolved in 200 parts by volume of hot hexane
  5. filtrationthis mixture was then filtered
  6. temperaturecooled

출처 및 근거

ORD 기록
ord-6a1780e8a4d341cf88cffeb2aab9ad45
출처 데이터셋
uspto-grants-1995_11
특허 번호
US05464830

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