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Water → HCID 13564978, 화합물

HRID 236574
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HRID 236574 반응식
[CH3:1][C:2]1[NH:3][C:4]([CH3:24])=[C:5]([C:18]([O:20][CH2:21][CH2:22][OH:23])=[O:19])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[C:7]=1[N+:8]([O-:10])=[O:9].[OH2:25].N1[CH:31]=[CH:30]C=CC=1>C(OC(=O)C)(=O)C>[CH3:1][C:2]1[NH:3][C:4]([CH3:24])=[C:5]([C:18]([O:20][CH2:21][CH2:22][O:23][C:30](=[O:25])[CH3:31])=[O:19])[CH:6]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])[C:7]=1[N+:8]([O-:10])=[O:9]
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참가 물질

5

반응물 3

HCID 962WaterHCID 1049PyridineHCID 13564994beta-Hydroxyethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylate

생성물 1

HCID 13564978HCID 13564978, 화합물

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

1 g of β-hydroxyethyl 1,4-dihydro-2,6-dimethyl-3-nitro-4-(2-chlorophenyl)-pyridine-5-carboxylate is stirred overnight in a mixture of 15 ml of pyridine and 15 ml of acetic anhydride. The mixture is poured into water and extracted with ethyl acetate and the extract is washed with 1 N HCl, water, sodium bicarbonate solution and water again, dried and concentrated. The evaporation residue is crystallized with ethanol, filtered off with suction and washed with ethanol. 800 mg of a yellow-coloured compound of melting point 166° C. which is identical to the compound from Preparation Example 1, process variant A are obtained.

후처리

  1. extractionextracted with ethyl acetate
  2. washthe extract is washed with 1 N HCl, water, sodium bicarbonate solution and water again
  3. customdried
  4. concentrationconcentrated
  5. customThe evaporation residue is crystallized with ethanol
  6. filtrationfiltered off with suction
  7. washwashed with ethanol
  8. custom800 mg of a yellow-coloured compound of melting point 166° C. which is identical to the compound from Preparation Example 1, process variant
  9. customA are obtained

출처 및 근거

ORD 기록
ord-df9ca2833d9c4455885a22cbcdb68161
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04645775

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