m-Chloroperbenzoic acid → 3-Hydroxymethyl-10,11-dihydrodibenzo[b,f]thiepin-5-oxide

HRID 1732352ノート

反応式

HRID 1732352 の反応式
[OH:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH2:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[S:8][C:7]=2[CH:17]=1.ClC1C=CC=C(C(OO)=[O:26])C=1.[OH-].[Ca+2].[OH-]>C(Cl)Cl>[OH:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[CH2:12][CH2:11][C:10]3[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=3[S:8](=[O:26])[C:7]=2[CH:17]=1

参加物

5

反応物 3

HCID 70297m-Chloroperbenzoic acidHCID 6093208Calcium HydroxideHCID 202555023-Hydroxymethyl-10,11-dihydrodibenzo[b,f]thiepin

生成物 1

HCID 202555043-Hydroxymethyl-10,11-dihydrodibenzo[b,f]thiepin-5-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

Dissolve 2 gm. of 3-hydroxymethyl-10,11-dihydrodibenzo[b,f]thiepin in 200 ml. of methylene chloride at room temperature. Add 1.7 gm. of m-chloroperbenzoic acid. Stir at room temperature for 2 hours. Add 4 gm. of calcium hydroxide and 50 ml. of methylene chloride. Continue stirring for 15 minutes. Filter through celite and evaporate the filtrate to dryness. Crystallize the residue from toluene to obtain the title product (m.p., 144°-146° C.).

後処理

  1. dissolutionDissolve 2 gm
  2. customat room temperature
  3. additionAdd 1.7 gm
  4. additionAdd 4 gm
  5. stirringContinue stirring for 15 minutes
  6. filtrationFilter through celite
  7. customevaporate the filtrate to dryness
  8. customCrystallize the residue from toluene

出典と根拠

ORDレコード
ord-a2fcbbd47c5647fcaf3aff6a31e97715
出典データセット
uspto-grants-1980_12
特許番号
US04237160

反応ノート

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