Hydrochloric Acid → [(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-(aminomethylene)-2,6-diisopropyl-phenyl ester

HRID 2289690ノート

反応式

HRID 2289690 の反応式
[C:1]([C:3]1[CH:8]=[C:7]([CH:9]([CH3:11])[CH3:10])[C:6]([O:12][S:13](=[O:34])(=[O:33])[NH:14][C:15](=[O:32])[CH2:16][C:17]2[C:22]([CH:23]([CH3:25])[CH3:24])=[CH:21][C:20]([CH:26]([CH3:28])[CH3:27])=[CH:19][C:18]=2[CH:29]([CH3:31])[CH3:30])=[C:5]([CH:35]([CH3:37])[CH3:36])[CH:4]=1)#[N:2].[H][H].Cl>N.C(OCC)C.[Ni]>[NH2:2][CH:1]=[C:3]1[CH:4]=[C:5]([CH:35]([CH3:36])[CH3:37])[C:6]([O:12][S:13](=[O:33])(=[O:34])[NH:14][C:15](=[O:32])[CH2:16][C:17]2[C:18]([CH:29]([CH3:30])[CH3:31])=[CH:19][C:20]([CH:26]([CH3:27])[CH3:28])=[CH:21][C:22]=2[CH:23]([CH3:25])[CH3:24])=[C:7]([CH:9]([CH3:11])[CH3:10])[CH2:8]1

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 10165237[(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-cyano-2,6-diisopropyl-phenyl esterHCID 178418361HCID 178418361、化合物

生成物 1

HCID 53945870[(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-(aminomethylene)-2,6-diisopropyl-phenyl ester

試薬・触媒・溶媒 3

HCID 935Nickel触媒HCID 222Ammonia溶媒HCID 3283Diethyl Ether溶媒

実験手順

[(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-cyano-2,6-diisopropyl-phenyl ester (5.15 g, 9.8 mmol) was dissolved in 100 mL of methanolic ammonia and 2.0 g of Raney-nickel was added. The resulting mixture was stirred under 50 psi of hydrogen at room temperature for 20 hours. Filtered and concentrated the residue to give a dark solid. Suspended in diethyl ether and acidified with HCl gas. Concentrated in vacuo and neutralized the residue with saturated aqueous sodium bicarbonate. The resulting white suspension was used without further purification.

後処理

  1. filtrationFiltered
  2. concentrationconcentrated the residue
  3. customto give a dark solid
  4. concentrationConcentrated in vacuo
  5. customThe resulting white suspension was used without further purification

出典と根拠

ORDレコード
ord-c536a0f073004c3ea1f33876b293bad1
出典データセット
uspto-grants-2000_07
特許番号
US06093744

反応ノート

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