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

HRID 1732352노트

반응식

HRID 1732352 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-a2fcbbd47c5647fcaf3aff6a31e97715
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237160

반응 노트

불러오는 중…