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

HRID 275287

反応式

HRID 275287 の反応式
[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

参加物

6

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-435993d45ac542a7a51790e48c75e7bc
出典データセット
uspto-grants-1995_02
特許番号
US05393747

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