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Triethylamine → HCID 67539565、化合物

HRID 1192379
ノート
印刷プレビュー

反応式

HRID 1192379 の反応式
C(N(CC)CC)C.[C:8]([NH:15][C@@H:16]([C:25]([OH:27])=O)[CH2:17][C:18]1[CH:23]=[CH:22][C:21]([Cl:24])=[CH:20][CH:19]=1)([O:10][C:11]([CH3:14])([CH3:13])[CH3:12])=[O:9].Cl.Cl.[N:30]1([C:36]2[N:40]3[CH:41]=[CH:42][CH:43]=[CH:44][C:39]3=[N:38][CH:37]=2)[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1.ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[OH-].[Na+]>CN(C=O)C.O>[C:11]([O:10][C:8](=[O:9])[NH:15][C@H:16]([CH2:17][C:18]1[CH:19]=[CH:20][C:21]([Cl:24])=[CH:22][CH:23]=1)[C:25]([N:33]1[CH2:34][CH2:35][N:30]([C:36]2[N:40]3[CH:41]=[CH:42][CH:43]=[CH:44][C:39]3=[N:38][CH:37]=2)[CH2:31][CH2:32]1)=[O:27])([CH3:12])([CH3:13])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 7018791N-Boc-4-chloro-D-phenylalanineHCID 67539435853680-34-9

生成物 1

HCID 67539565
HCID 67539565、化合物
収率 66.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Triethylamine (0.30 mL, 2.18 mmol) was added to a solution of (R)—N-Boc-4-chlorophenylalanine (392 mg, 1.31 mmol), 3-piperazin-1-yl-imidazo[1,2-a]pyridine dihydrochloride (300 mg, 1.09 mmol), and 1-hydroxybenzotriazole (177 mg, 1.31 mmol) in DMF (5 mL) followed by the addition of 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (251 mg, 1.31 mmol) in a single portion. After being stirred for 12 hours, the mixture was diluted with H2O, basified to pH 12 with 1.0 M NaOH, and extracted with DCM. The DCM extracts were dried (Na2SO4), filtered, and concentrated in vacuo. The residue was chromatographed (SiO2) using DCM:Et2O (1:1) followed by 10% MeOH/DCM as eluent to give (R)-[1-(4-chlorobenzyl)-2-(4-imidazo[1,2-a]pyridin-3-yl-piperazin-1-yl)-2-oxo-ethyl]-carbamic acid tert-butyl ester (350 mg).

後処理

  1. extractionextracted with DCM
  2. dry with materialThe DCM extracts were dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed (SiO2)

出典と根拠

ORDレコード
ord-026e8f60d1ea4608b75be9c155ede11e
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08680114B2

反応ノート

読み込み中…

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