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

HRID 435192

반응식

HRID 435192 반응식
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]

참가 물질

8

반응물 4

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 7911MalonamideHCID 13838Hexamethyldisilazane

생성물 1

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

시약·촉매·용매 3

HCID 5143Saccharin촉매HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-26864b483c4f4499ba9816be3ef8ef45
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04400509

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