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Ethanol → HCID 18768043, 화합물

HRID 480021
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HRID 480021 반응식
S(S([O-])=O)([O-])=O.[Na+].[Na+].[NH:9]([C:16]1[C:21]([Br:22])=[CH:20][N:19]=[C:18]([NH:23][C:24]2[CH:29]=[CH:28][C:27]([N+:30]([O-])=O)=[CH:26][CH:25]=2)[N:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.C(O)C>O>[NH2:30][C:27]1[CH:28]=[CH:29][C:24]([NH:23][C:18]2[N:17]=[C:16]([NH:9][C:10]3[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=3)[C:21]([Br:22])=[CH:20][N:19]=2)=[CH:25][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 702EthanolHCID 24489Sodium DithioniteHCID 18768056HCID 18768056, 화합물

생성물 1

HCID 18768043HCID 18768043, 화합물수율 70.2%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Sodium hydrosulphite (9.5 g, 54.5 mmol) was added over 30 minutes to a stirred solution of anilino-5-bromo-2-(4-nitroanilino)pyrimidine (Method 39; 7.0 g, 18.2 mmol) in a hot mixture of ethanol and water (1:1, 100 ml). The resulting suspension was stirred for a further two hours and insoluble material was removed by filtration. The filtrate was concentrated and the residue was partitioned between 1M aqueous sodium hydroxide (50 ml), and DCM (100 ml). The organic layer was separated, washed with water (2×10 ml) and dried. Volatile material was removed by evaporation to give the product (4.55 g, 70%). MS (MH+): 356, 358.

후처리

  1. custominsoluble material was removed by filtration
  2. concentrationThe filtrate was concentrated
  3. customthe residue was partitioned between 1M aqueous sodium hydroxide (50 ml), and DCM (100 ml)
  4. customThe organic layer was separated
  5. washwashed with water (2×10 ml)
  6. customdried
  7. customVolatile material was removed by evaporation

출처 및 근거

ORD 기록
ord-41e7102dc5f44e05bd0fd4c31727f8ae
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649608B2

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