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Dichloromethane → HCID 86660158, 화합물

HRID 514780
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HRID 514780 반응식
[CH2:1]([NH:3][S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N+:13]([O-:15])=[O:14])(=[O:6])=[O:5])[CH3:2].[Br:16][CH2:17][CH2:18][CH2:19]Br.[H-].[Na+].C(Cl)Cl>CN(C=O)C>[Br:16][CH2:17][CH2:18][CH2:19][N:3]([CH2:1][CH3:2])[S:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[N+:13]([O-:15])=[O:14])(=[O:5])=[O:6]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 80011,3-DibromopropaneHCID 24758Sodium hydrideHCID 744706N-ethyl-2-nitrobenzene-1-sulfonamide

생성물 1

HCID 86660158HCID 86660158, 화합물수율 82%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Compound 63 (7.8 g, 33.9 mmol) was dissolved in DMF (100 mL). 1,3-Dibromopropane (35 mL, 343.0 mmol) and then in portions NaH (2.7 g, 67.5 mmol) were added, whereupon the temperature rose to 50-60° C. The reaction mixture was stirred at this temperature for 1 h (TLC monitoring, CH2Cl2), carefully poured into ice/water mixture, and extracted with ethyl acetate. The extract was evaporated. The residue washed with hexane to remove the 1,3-dibromopropane. Compound 64 (9.7 g, 82%) was obtained as a viscous yellow oil.

후처리

  1. customrose to 50-60° C
  2. extractionextracted with ethyl acetate
  3. customThe extract was evaporated
  4. washThe residue washed with hexane
  5. customto remove the 1,3-dibromopropane

출처 및 근거

ORD 기록
ord-d98c8f7764bf4173b03841ebb898183c
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09108916B2

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