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Hydrogen Bromide → HCID 68902424, 화합물

HRID 1436417
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HRID 1436417 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([C:10](=O)[CH2:11][S:12][C:13]#[N:14])=[CH:6][CH:5]=1)([O-:3])=[O:2].[BrH:16].[OH-].[Na+].O>C(O)(=O)C>[Br:16][C:13]1[S:12][CH:11]=[C:10]([C:7]2[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=2)[N:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 260Hydrogen BromideHCID 962WaterHCID 14798Sodium HydroxideHCID 19884882-(4-Nitrophenyl)-2-oxoethyl thiocyanate

생성물 1

HCID 68902424HCID 68902424, 화합물수율 45%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

2-(4-Nitrophenyl)-2-oxoethyl thiocyanate (3.0 g; 15.4 mmol) and 50 mL of 30% HBr in acetic acid were stirred at room temperature under nitrogen overnight. The yellow paste was neutralized with 60 mL of 2N NaOH and 60 mL of H2O. The residue was collected by suction filtration. Purification of the residue on silica gel using a stepwise gradient of 5-50% ethyl acetate:hexane gave 2-bromo-4-(4-nitrophenyl)-1,3-thiazole (2.0 g, 45%), MS (ES) m/z 286[M+H]+.

후처리

  1. filtrationThe residue was collected by suction filtration
  2. customPurification of the residue on silica gel using a stepwise gradient of 5-50% ethyl acetate

출처 및 근거

ORD 기록
ord-035e9b0379814ac0b00bc3e4b82f5040
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07618990B2

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