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Ammonium Chloride → 2-Bromobenzyl methyl sulfide

HRID 1588894
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HRID 1588894 반응식
[CH3:1][S-:2].[Li+].[Br:4][C:5]1[CH:12]=[CH:11][CH:10]=[CH:9][C:6]=1[CH2:7]Br.[NH4+].[Cl-]>C(O)C.C1COCC1>[CH3:1][S:2][CH2:7][C:6]1[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=1[Br:4]
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참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 769652-Bromobenzyl bromideHCID 11018798HCID 11018798, 화합물

생성물 1

HCID 41081382-Bromobenzyl methyl sulfide수율 90.7%

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

To a stirred solution of lithium thiomethoxide (82.19 mmol, generated from n-BuLi and methylmercaptan) in 130 ml of ethanol/THF (2:3) 2-bromobenzylbromide (12.54 g, 50.17 mmol) was added. After 1 h of reflux 30 ml of a saturated aqueous NH4Cl solution was added. The mixture was concentrated and extracted with ether The organic phase was washed with water and dried with MgSO4. After evaporation the crude product was distilled to give a clear liquid of o-bromobenzyl methyl sulfide 9.88 g (89%).

후처리

  1. concentrationThe mixture was concentrated
  2. extractionextracted with ether The organic phase
  3. washwas washed with water
  4. dry with materialdried with MgSO4
  5. customAfter evaporation the crude product
  6. distillationwas distilled

출처 및 근거

ORD 기록
ord-4bc70bd1dd274ada8534b06842a83eca
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05223591

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