Ammonia → Malonyldiamide, N,N'-bis(trimethylsilyl)-

HRID 435192ノート

反応式

HRID 435192 の反応式
C[Si](C)(C)[NH:3][Si:4]([CH3:7])([CH3:6])[CH3:5].[C:10]([NH2:16])(=[O:15])[CH2:11][C:12](N)=[O:13].S(=O)(=O)(O)O.N>S1(C2C(=CC=CC=2)C(=O)N1)(=O)=O.N1C=CC=CC=1.C(OCC)(=O)C>[CH3:5][Si:4]([CH3:7])([CH3:6])[NH:16][C:10](=[O:15])[CH2:11][C:12]([NH:3][Si:4]([CH3:5])([CH3:6])[CH3:7])=[O:13]

参加物

8

反応物 4

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 7911MalonamideHCID 13838Hexamethyldisilazane

生成物 1

HCID 554458Malonyldiamide, N,N'-bis(trimethylsilyl)-収率 99,004.203%

試薬・触媒・溶媒 3

HCID 5143Saccharin触媒HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

7.5 ml (36 mmoles) of hexamethyldisilazane were added to a refluxing mixture of 3.06 g (0.03 mmole) of malonamide, 18.3 mg (0.1 mmole) of saccharin, 50 ml of ethyl acetate and 5 ml of pyridine and by titrating with 1 N sulfuric acid the ammonia evolved, it was found that 30 mmoles were expelled after refluxing for one hour. Volatile material was vacuum evaporated and the residue, which crystallized upon standing, was dried in vacuo to obtain 7.32 g (99%) of N,N'-bis-(trimethylsilyl)-malonamide melting at 72°-76° C. NMR Spectrum (CDCl3): Δ0.24 (s, 18H); 3.20 (s, 2H); 6.5 (broad, 2H).

後処理

  1. temperatureafter refluxing for one hour
  2. customevaporated
  3. customthe residue, which crystallized
  4. customwas dried in vacuo

出典と根拠

ORDレコード
ord-26864b483c4f4499ba9816be3ef8ef45
出典データセット
uspto-grants-1983_08
特許番号
US04400509

反応ノート

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