Methanol → HCID 71087465、化合物

HRID 631989ノート

反応式

HRID 631989 の反応式
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

参加物

6

反応物 4

HCID 887MethanolHCID 1049PyridineHCID 76284hydroxylamine-O-sulfonic acidHCID 86674739HCID 86674739、化合物

生成物 1

HCID 71087465HCID 71087465、化合物収率 97.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-efe16bb89fc54475b89ed7b64def5e85
出典データセット
uspto-grants-2016_04
特許番号
US09321727B2

反応ノート

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