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Bromine → methyl-4-(10,11-dibromo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine hydrobromide

HRID 1288441
ノート
印刷プレビュー

反応式

HRID 1288441 の反応式
[BrH:1].[CH3:2][N:3]1[CH2:8][CH2:7][C:6](=[C:9]2[C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH:13]=[CH:12][C:11]3[CH:20]=[CH:21][CH:22]=[CH:23][C:10]2=3)[CH2:5][CH2:4]1.[Br:24]Br>C(O)(=O)C>[BrH:1].[CH3:2][N:3]1[CH2:8][CH2:7][C:6](=[C:9]2[C:10]3[CH:23]=[CH:22][CH:21]=[CH:20][C:11]=3[CH:12]([Br:1])[CH:13]([Br:24])[C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]2=3)[CH2:5][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 24408BromineHCID 215022761-Methyl-4-(5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine hydrobromide

生成物 1

HCID 20328344methyl-4-(10,11-dibromo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)piperidine hydrobromide

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

実験手順

1-Methyl-4-(5H-dibenzo[a,d]cyclohepten-5-ylidene)-piperidine hydrobromide, 18.40 g. (0.05 mole) is dissolved with warming in 750 ml. of glacial acetic acid. This solution is cooled to room temperature and 8.0 g., 2.6 ml., (0.05 mole) of bromine dissolved in 75 ml. of glacial acetic acid is added dropwise with stirring. After completion of the addition the mixture is stirred overnight. The crystals are collected, washed with a small amount of cold glacial acetic acid, then with dry ether, and then dried for 2 hours in a vacuum oven at 70° C. to give 1-methyl-4-(10,11-dibromo-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-ylidene)-piperidine hydrobromide. Recrystallization from acetonitrile gives an analytical sample, m.p. 185°-186° C.

後処理

  1. dissolution(0.05 mole) is dissolved
  2. temperaturewith warming in 750 ml
  3. additionAfter completion of the addition the mixture
  4. stirringis stirred overnight
  5. customThe crystals are collected
  6. washwashed with a small amount of cold glacial acetic acid
  7. dry with materialwith dry ether, and then dried for 2 hours in a vacuum oven at 70° C.

出典と根拠

ORDレコード
ord-60698279b38d4439bf5d1d955d31fce2
出典データセット
uspto-grants-1976_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03988342

反応ノート

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