Methanethiol → HCID 21320299, 화합물

HRID 262227노트

반응식

HRID 262227 반응식
[Br:1][C:2]1[O:3][C:4]2[CH:16]=[CH:15][C:14]([CH2:17][S:18][CH3:19])=[CH:13][C:5]=2[C:6]=1[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.BrC1[O:22]C2C=CC(CBr)=CC=2C=1C1C=CC=CC=1.CS.ClC1C=CC=C(C(OO)=O)C=1>C(Cl)(Cl)Cl>[Br:1][C:2]1[O:3][C:4]2[CH:16]=[CH:15][C:14]([CH2:17][S:18]([CH3:19])=[O:22])=[CH:13][C:5]=2[C:6]=1[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

참가 물질

6

반응물 4

HCID 878MethanethiolHCID 70297m-Chloroperbenzoic acidHCID 20333828HCID 20333828, 화합물HCID 21320278HCID 21320278, 화합물

생성물 1

HCID 21320299HCID 21320299, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

To a stirred, cold solution of 7.8 g. of 2-bromo-5-methylthiomethyl-3-phenylbenzofuran (prepared by reacting 2-bromo-5-bromomethyl-3-phenylbenzofuran with methyl mercaptan according to the procedure of Example 18 hereof) in 100 ml. of chloroform is added dropwise 4.73 g. of 3-chloroperbenzoic acid in chloroform at 0° C. After three hours an addition 0.3 g. of the peracid is added and 30 minutes later the solution is washed with cold 5 percent sodium hydroxide solution, then with saturated sodium chloride solution and dried. Evaporation provides a residue which is recrystallized from a chloroform-hexane mixture to provide 2-bromo-5-methylsulfinylmethyl-3-phenylbenzofuran. The structural assignment is confirmed by infrared and nuclear magnetic resonance spectral analysis.

후처리

  1. customat 0° C
  2. additionAfter three hours an addition 0.3 g
  3. washis washed with cold 5 percent sodium hydroxide solution
  4. dry with materialwith saturated sodium chloride solution and dried
  5. customEvaporation
  6. customprovides a residue which
  7. customis recrystallized from a chloroform-hexane mixture

출처 및 근거

ORD 기록
ord-7fddbe14c64848fca286907601e41992
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04153716

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