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Benzyl mercaptan → HCID 20475694, 화합물

HRID 905221
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HRID 905221 반응식
Cl[C:2]1[N:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1.[CH:11]1[CH:16]=[CH:15][C:14]([CH2:17][SH:18])=[CH:13][CH:12]=1.CC[O-].[Na+]>C(O)C>[CH2:17]([S:18][C:2]1[N:7]=[C:6]([CH3:8])[C:5]([Br:9])=[C:4]([CH3:10])[N:3]=1)[C:14]1[CH:15]=[CH:16][CH:11]=[CH:12][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7509Benzyl mercaptanHCID 2723922Sodium ethoxideHCID 125019865-Bromo-2-chloro-4,6-dimethylpyrimidine

생성물 1

HCID 20475694HCID 20475694, 화합물수율 94%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2-Chloro-4,6-dimethyl-5-bromopyrimidine (10 mmol) was added to a solution of benzylthiol (11 mmol) and 0.138 M NaOEt in ethanol (80 ml). The mixture was stirred at room temperature for 70 min and then heated under reflux for 40 min. The solvent was then distilled off, the residue extracted with chloroform (50 ml), the chloroform solution washed with 2 M NaOH and the dried (MgSO4) solution evaporated to leave the sulfide which was purified by distillation; yield 94%, b.p. 232°-234° C./15 mmHg. 1H NMR (Cl3CF): δ2.50 (Me-4, Me-6), 4.26 (CH2), 7.20 (Ph).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 40 min
  3. distillationThe solvent was then distilled off
  4. extractionthe residue extracted with chloroform (50 ml)
  5. washthe chloroform solution washed with 2 M NaOH
  6. dry with materialthe dried (MgSO4) solution
  7. customevaporated

출처 및 근거

ORD 기록
ord-eb44e0c4bd974b77bee37b95899a92ad
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04423047

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