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Hydrochloric Acid → HCID 20622811, 화합물

HRID 2121220
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HRID 2121220 반응식
C[O:2][C:3](=O)[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][NH:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[CH3:18])=[CH:6][C:5]=1[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[OH-].[Li+].Cl.Cl.[CH3:30][O:31][C:32](=[O:39])[C@H:33]([CH2:35][CH2:36][S:37][CH3:38])[NH2:34].ON1C(=O)C2C=CC=CC=2N=N1.CN(C)CCCN=C=NCC>CO.C(OCC)(=O)C.N1C=CC=CC=1.C1COCC1>[CH3:30][O:31][C:32](=[O:39])[C@H:33]([CH2:35][CH2:36][S:37][CH3:38])[NH:34][C:3](=[O:2])[C:4]1[CH:9]=[CH:8][C:7]([CH2:10][NH:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[CH3:18])=[CH:6][C:5]=1[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 6

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 730263-hydroxy-1,2,3-benzotriazin-4(3H)-oneHCID 11435579L-Methionine, methyl ester, hydrochlorideHCID 54568565HCID 54568565, 화합물

생성물 1

HCID 20622811
HCID 20622811, 화합물

시약·촉매·용매 4

HCID 887Methanol용매HCID 1049Pyridine용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of the product of Example 280B (446 mg, 1.3 mmol) and aqueous saturated lithium hydroxide (3 mL) in methanol (5 mL) was heated at 60° C. for 15 hours. The reaction mixture was then neutralized with hydrogen chloride (4 N in dioxane, 5 mL). The reaction mixture was concentrated in vacuo to dryness. To the residue was added sequentially L-methionine methyl ester hydrochloride (311 mg, 1.56 mmol), 3-hydroxy 1,2,3-benzotriazin-4(3H)-one (318 mg, 1.95 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodimide (374 mg, 1.95 mmol), THF (10 mL) and pyridine (1 mL). After 15 hours, the reaction mixture was diluted with ethyl acetate, washed with water and brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue was then purified by column chromatography (ethyl acetate) to give the title compound.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo to dryness
  2. washwashed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was then purified by column chromatography (ethyl acetate)

출처 및 근거

ORD 기록
ord-d30f093b1e4c4bffbabaa70415dca66f
출처 데이터셋
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06693123B2

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