Acetic Acid → HCID 68279118, 화합물

HRID 338791

반응식

HRID 338791 반응식
C(O)(=O)C.[NH2:5][C:6]1[CH:11]=[C:10]([Cl:12])[CH:9]=[CH:8][C:7]=1[SH:13].[OH:14][C:15]1[CH:16]=[C:17]([CH:20]=[C:21]([OH:23])[CH:22]=1)[CH:18]=O.C([O-])(=O)C.[Na+]>O.C(OCC)(=O)C>[Cl:12][C:10]1[CH:9]=[CH:8][C:7]2[S:13][C:18]([C:17]3[CH:20]=[C:21]([OH:23])[CH:22]=[C:15]([OH:14])[CH:16]=3)=[N:5][C:6]=2[CH:11]=1

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 120002-Amino-4-chlorobenzenethiolHCID 943653,5-DihydroxybenzaldehydeHCID 517045Sodium Acetate

생성물 1

HCID 68279118HCID 68279118, 화합물수율 52.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

In an acetic acid (0.6 mL) solvent, a mixture including 2-amino-4-chlorobenzenethiol (100 mg, 0.44 mmol), 3,5-dihydroxybenzaldehyde (60 mg, 0.44 mmol), and sodium acetate (107 mg, 1.30 mmol) was refluxed for 7 hours. After cooling, the reaction mixture was distributed between ethyl acetate and water, and an organic layer was dried by using MgSO4, filtered, and evaporated under reduced pressure. The residual was purified by silica gel column chromatography using hexane and ethyl acetate (2:1) as a developer to obtain a solid Compound 90 (64.2 mg, 34.7%).

후처리

  1. temperaturewas refluxed for 7 hours
  2. temperatureAfter cooling
  3. customan organic layer was dried
  4. filtrationfiltered
  5. customevaporated under reduced pressure
  6. customThe residual was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-00de919081644ab5a0b3412e0df89b4d
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889881B2

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