Sodium Glycinate → n-(5'-Chloro-4'-methyl-2'-nitrophenyl)glycine sodium salt

HRID 1068600

반응식

HRID 1068600 반응식
[Cl:1][C:2]1[CH:7]=[C:6](F)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[CH3:12].[NH2:13][CH2:14][C:15]([O-:17])=[O:16].[Na+:18]>CN(C=O)C.O>[Na+:18].[Cl:1][C:2]1[C:3]([CH3:12])=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([NH:13][CH2:14][C:15]([O-:17])=[O:16])[CH:7]=1

참가 물질

5

반응물 2

HCID 4684308Sodium GlycinateHCID 101039792-Chloro-4-fluoro-5-nitrotoluene

생성물 1

HCID 21190047n-(5'-Chloro-4'-methyl-2'-nitrophenyl)glycine sodium salt

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
70 °C

실험 절차

To a stirred solution of 2-chloro-4-fluoro-5-nitrotoluene (2.080 g, 10.97 mmol, as prepared above) in DMF (11.0 mL) at 70° C., was added dropwise, a solution of sodium glycinate (1.065 g, 10.97 mmol, Aldrich, used as received) in water (11.0 mL). The resulting suspension was stirred overnight at 70° C., cooled to room temperature, and the resulting red solid was filtered, washed with acetone (35 mL), and dried under vacuum to give 1.005 g (37%) of the pure (1H NMR) title compound as a red powder, 1H NMR (DMSO-d6): δ 2.184 (s, 3H), 3.396 (d, 2H, J=4.2 Hz), 6.852 (s, 1H), 7.991 (s, 1H), 8.671 (s, 1H).

후처리

  1. temperaturecooled to room temperature
  2. filtrationthe resulting red solid was filtered
  3. washwashed with acetone (35 mL)
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-5362c0a9fe274957865a5249b02ff81b
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06251903B1

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