Methanol → HCID 71087465, 화합물

HRID 927375노트

반응식

HRID 927375 반응식
C[N:2](C)[C:3](=[N:5][C:6](=[S:18])[C:7]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:9])[CH3:8])[CH3:4].NOS(O)(=O)=O.N1C=CC=CC=1.CO>C(O)C>[CH3:4][C:3]1[N:5]=[C:6]([C:7]([NH:10][C:11](=[O:17])[O:12][C:13]([CH3:16])([CH3:15])[CH3:14])([CH3:9])[CH3:8])[S:18][N:2]=1

참가 물질

6

반응물 4

HCID 887MethanolHCID 1049PyridineHCID 76284hydroxylamine-O-sulfonic acidHCID 86674739HCID 86674739, 화합물

생성물 1

HCID 71087465HCID 71087465, 화합물수율 97.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of tert-butyl 1-(1-(dimethylamino)ethylideneamino)-2-methyl-1-thioxopropan-2-ylcarbamate (2.9 g, 10 mmol), hydroxylamine-O-sulfonic acid (CAN 2950-43-8, 1.37 g, 12 mmol), pyridine (1.6 g, 20.2 mmol) and methanol (4 mL) in ethanol (20 mL) was stirred at room temperature for 2 h. After evaporation of solvents, the residue was diluted with ethyl acetate (40 mL) and water (40 mL). The organic layer was washed with brine (40 mL), dried over anhydrous sodium sulfate and concentrated to give crude product (2.5 g, 96%) as yellow oil. The product was used directly in the next step without further purification; MS (EI): m/e 258.2 [M+H]+.

후처리

  1. customAfter evaporation of solvents
  2. additionthe residue was diluted with ethyl acetate (40 mL) and water (40 mL)
  3. washThe organic layer was washed with brine (40 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0f2f1b55978b44f9a282793074d2c705
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290451B2

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