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

HRID 2289690노트

반응식

HRID 2289690 반응식
[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

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 935Nickel촉매HCID 222Ammonia용매HCID 3283Diethyl Ether용매

실험 절차

[(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.

후처리

  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

출처 및 근거

ORD 기록
ord-c536a0f073004c3ea1f33876b293bad1
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06093744

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