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Hydrochloric Acid → HCID 20622811、化合物

HRID 2121220
ノート
印刷プレビュー

反応式

HRID 2121220 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 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、化合物

生成物 1

HCID 20622811
HCID 20622811、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-d30f093b1e4c4bffbabaa70415dca66f
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693123B2

反応ノート

読み込み中…

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