Dichloromethane → HCID 57378117, 화합물

HRID 511907노트

반응식

HRID 511907 반응식
C(N(CC)CC)C.[C:8]([N:15]1[CH:19]=[CH:18]N=C1)(N1C=CN=C1)=[S:9].C(Cl)Cl.NC1C=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1>C(OCC)(=O)C>[N:15]([C:19]1[CH:18]=[CH:31][C:27]([C:28]([OH:30])=[O:29])=[C:26]([N+:33]([O-:35])=[O:34])[CH:25]=1)=[C:8]=[S:9]

참가 물질

6

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 802641,1'-ThiocarbonyldiimidazoleHCID 2357134-Amino-2-nitrobenzoic Acid

생성물 1

HCID 57378117HCID 57378117, 화합물수율 89%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Triethylamine (55.8 μL, 0.4 mmol) and thiocarbonyldiimidazole (46.3 mg, 0.26 mmol) were added to a methylene chloride solution (0.4 mL) of 4-amino-2-nitrobenzoic acid (36.4 mg, 0.2 mmol) at room temperature, followed by stirring at room temperature for 10 minutes. The reaction mixture was dissolved in ethyl acetate and washed with 1 M hydrochloric acid, the organic layer was separated, and then the organic layer was dried over magnesium sulfate. Thereafter, filtration and concentration under reduced pressure to dryness were carried out to obtain 4-isothiocyanato-2-nitrobenzoic acid as a colorless solid (40 mg, yield: 89%, HPLC purity: 96.4%)

후처리

  1. washwashed with 1 M hydrochloric acid
  2. customthe organic layer was separated
  3. dry with materialthe organic layer was dried over magnesium sulfate
  4. filtrationThereafter, filtration and concentration under reduced pressure to dryness

출처 및 근거

ORD 기록
ord-3ec28024c9bd4081b8104eea24de2c4b
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09102602B2

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