Sodium Hydroxide → HCID 178418894, 화합물

HRID 10733

반응식

HRID 10733 반응식
[CH3:1][O:2][C:3]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:4]=1[C:5]([NH:7][NH:8][C:9]([NH:11][CH2:12][CH:13]([CH3:15])[CH3:14])=[S:10])=O.[OH-].[Na+]>C(O)C>[CH3:1][O:2][C:3]1[CH:19]=[C:18]([O:20][CH3:21])[CH:17]=[CH:16][C:4]=1[C:5]1[N:11]([CH2:12][CH:13]([CH3:15])[CH3:14])[C:9]([SH:10])=[N:8][N:7]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22084281-[(2,4-Dimethoxybenzoyl)amino]-3-(2-methylpropyl)thiourea

생성물 1

HCID 178418894HCID 178418894, 화합물수율 21.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ex-109C: A solution of 1-(2,4-dimethoxy-benzoyl)amino-3-isobutyl-thiourea (Ex-109B, 0.5 g, 1.61 mmol) and sodium hydroxide (0.999M, 4.8 mL, 4.8 mmol) in ethanol (30 mL) was refluxed for one day. The solvent was removed under reduced pressure and the residue redissolved in ethyl acetate. The solution of ethyl acetate was washed with water and brine, dried over sodium sulfate, and concentrated to give 5-(2,4-dimethoxy-phenyl)-4-isobutyl-4H-[1,2,4]triazole-3-thiol (0.1 g). Additional product (0.36 g, 98% overall) was obtained by extracting the water wash with dichloromethane and a mixture of isopropyl alcohol (33%, v/v, in dichloromethane). 1H NMR (CDCl3) δ 10.82 (bs, 1H), 7.24 (d, J=8.1 Hz, 1H), 6.56 (dd, J=8.1, 2.4 Hz, 1H), 6.51 (d, J=2.4 Hz, 1H), 3.85 (s, 3H), 3.77 (s, 3H), 3.72 (d, J=6.7 Hz, 2H), 2.17–2.08 (m, 1H), 0.70 (d, J=6.7 Hz, 6H).

후처리

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue redissolved in ethyl acetate
  3. washThe solution of ethyl acetate was washed with water and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0fa6753b39494df987413a4807ef9f7e
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07094801B2

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