Dichloromethane → 2-(3-Methoxybenzyl)benzenethiol

HRID 1158204노트

반응식

HRID 1158204 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[S:17]CC2C(OC)=CC(OC)=CC=2OC)O)[CH:6]=[CH:7][CH:8]=1.C([SiH](CC)CC)C.C(O)(C(F)(F)F)=O.C(Cl)Cl>C(OC(=O)C)C.CCCCCC.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[CH:7][CH:8]=1)[CH2:9][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[SH:17]

참가 물질

7

반응물 4

HCID 6344DichloromethaneHCID 6422Trifluoroacetic acidHCID 12052TriethylsilaneHCID 68643652(3-Methoxyphenyl)(2-(2,4,6-trimethoxybenzylthio)phenyl)methanol

생성물 1

HCID 686436202-(3-Methoxybenzyl)benzenethiol수율 77%

시약·촉매·용매 2

HCID 962Water용매HCID 21226206Ethyl acetate hexane용매

실험 절차

0.288 g (3-methoxyphenyl)(2-(2,4,6-trimethoxybenzylthio)phenyl)methanol (K) (0.68 mmol) was treated with a solution of triethylsilane:TFA:DCM 0.3 ml:1 ml: 10 ml. The mixture was stirred overnight at ambient temperature before the addition of water. The mixture was extracted with DCM, brine, dried over magnesium sulfate and concentrated. Flash silica chromatography (hexane ethyl acetate 90:10) afforded 0.12 g product (0.52 mmol, 77% yield).

후처리

  1. extractionThe mixture was extracted with DCM, brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2d9b18eafa33450fbb9d807198ebb6cf
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807713B2

반응 노트

불러오는 중…