Water → HCID 131733986、化合物

HRID 712353ノート

反応式

HRID 712353 の反応式
Br.[C:2]([S:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=1)(=[NH:4])[NH2:3].[C:16]([O-])(=O)[CH3:17].[NH4+].C([N:23]=[C:24]=[O:25])C.O>CN(C=O)C>[CH2:16]([N:13]([CH2:10][CH3:11])[C:24]([NH2:23])=[O:25])[CH3:17].[N+:13]([C:10]1[CH:11]=[CH:12][C:7]([CH2:6][S:5][C:2](=[NH:3])[NH2:4])=[CH:8][CH:9]=1)([O-:15])=[O:14]

参加物

6

反応物 4

HCID 962WaterHCID 8022Ethyl isocyanateHCID 116350Pseudourea, 2-(p-nitrobenzyl)-2-thio-, monohydrobromideHCID 517165Ammonium Acetate

生成物 1

HCID 131733986HCID 131733986、化合物収率 41%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 4-nitrobenzyl carbamimidothioate hydrobromide (2.5 g, 8.55 mmol) in DMF (10 mL) was added aqueous buffer solution of ammonium acetate (pH ˜7, 4.0 mL) followed by addition of ethyl isocyanate (10 mL. 85.57 mmol) at rt and the mixture stirred at rt for 48 h. After completion of reaction (by TLC), water (10 mL) was added and a white precipitate formed. The reaction mixture was filtered and solid was washed with water to obtain the desired product as white solid (1.40 g, 41%). MS: 354.18 [M+H]+

後処理

  1. additionwas added
  2. customa white precipitate formed
  3. filtrationThe reaction mixture was filtered
  4. washsolid was washed with water

出典と根拠

ORDレコード
ord-2a107e64ce68453ea23c0c90efdfd565
出典データセット
uspto-grants-2015_11
特許番号
US09181234B2

反応ノート

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