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Hydrochloric Acid → 1-(3-Nitro-2-pyridinyl)-4-carbobenzoxypiperazine-2-carboxylic acid

HRID 1390350
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HRID 1390350 반응식
Cl.[C:2]([N:12]1[CH2:17][CH2:16][NH:15][CH:14]([C:18]([OH:20])=[O:19])[CH2:13]1)([O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[O:3].Cl[C:22]1[C:27]([N+:28]([O-:30])=[O:29])=[CH:26][CH:25]=[CH:24][N:23]=1.C(N(CC)CC)C.Cl>O.CS(C)=O>[N+:28]([C:27]1[C:22]([N:15]2[CH2:16][CH2:17][N:12]([C:2]([O:4][CH2:5][C:6]3[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=3)=[O:3])[CH2:13][CH:14]2[C:18]([OH:20])=[O:19])=[N:23][CH:24]=[CH:25][CH:26]=1)([O-:30])=[O:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 796132-Chloro-3-nitropyridineHCID 450726774-((Benzyloxy)carbonyl)piperazine-2-carboxylic acid hydrochloride

생성물 1

HCID 233397691-(3-Nitro-2-pyridinyl)-4-carbobenzoxypiperazine-2-carboxylic acid

시약·촉매·용매 2

HCID 679
Dimethyl Sulfoxide
용매
HCID 962Water용매

실험 절차

A solution of 6.0 g. of 4-carbobenzoxypiperazine-2-carboxylic acid hydrochloride, 3.3 g. of 2-chloro-3-nitropyridine and 15 ml. of triethyl amine in 100 ml. of dimethyl sulfoxide is heated at 60° with stirring for 18 hours. The mixture is diluted with 400 ml. of water, acidified to pH 3 with concentrated hydrochloric acid, and extracted repeatedly with ether. The combined ether extracts are dried (MgSO4) and concentrated. The residue is crystallized from ethyl acetate/heptane to give 6.3 g. of the title product, m.p. 145°-147°.

후처리

  1. additionThe mixture is diluted with 400 ml
  2. extractionextracted repeatedly with ether
  3. dry with materialThe combined ether extracts are dried (MgSO4)
  4. concentrationconcentrated
  5. customThe residue is crystallized from ethyl acetate/heptane
  6. customto give 6.3 g

출처 및 근거

ORD 기록
ord-db169d516f694ca6b21cdc3424535eec
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04138564

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