Methanol → Urea Urethane

HRID 1158186

反応式

HRID 1158186 の反応式
CC1C=CC(N=C=O)=CC=1[N:11]=[C:12]=[O:13].C[OH:15].[CH:16]1C([NH2:22])=CC=C(S(C2C=CC(N)=CC=2)(=O)=O)[CH:17]=1>C(C(C)=O)C>[NH2:22][C:12]([NH2:11])=[O:13].[NH2:11][C:12]([O:13][CH2:16][CH3:17])=[O:15]

参加物

5

反応物 3

HCID 887MethanolHCID 2955DapsoneHCID 11443Toluene 2,4-Diisocyanate

生成物 1

HCID 21585015Urea Urethane収率 269.1%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
60 °C

実験手順

To 17 g of 2,4-toluene diisocyanate was added 40 g of methyl ethyl ketone as a solvent, followed by adding dropwise thereto 3.8 g of methanol, and the reaction was carried out with stirring at 60° C. for 5 hours. Then, 9.9 g of 4,4′-diaminodiphenyl sulfone was added thereto, and the reaction was carried out with stirring at 60° C. for 4 hours. After completion of the reaction, the methyl ethyl ketone as solvent was removed by the use of an evaporator, and the residue was dried overnight in a vacuum to obtain 16 g of a urea-urethane composition as white crystals. The melting point of the white crystals was 169° C. In IR analysis on the crystals, characteristic peaks due to a urea-urethane compound appeared at 1660 cm−1 and 1740 cm−1. The content of the urea-urethane main constituent in the urea-urethane composition was 52% as measured by liquid chromatography.

後処理

  1. additionby adding dropwise
  2. stirringwith stirring at 60° C. for 4 hours
  3. customAfter completion of the reaction
  4. customthe methyl ethyl ketone as solvent was removed by the use of an evaporator
  5. customthe residue was dried overnight in a vacuum

出典と根拠

ORDレコード
ord-ff7ab37fd7344939a0c46a5e70468142
出典データセット
uspto-grants-2010_10
特許番号
US07807738B2

関連ノート

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