Triethylamine → HCID 21949151、化合物

HRID 2376834ノート

反応式

HRID 2376834 の反応式
N1([NH:7][C:8]([O:10][CH2:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[O:9])CCNCC1.[OH:18][C:19]([CH3:24])([CH3:23])[C:20](O)=[O:21].Cl.C(N=C=NCCCN(C)C)C.O.ON1C2C=CC=CC=2N=N1.[CH2:48]([N:50](CC)[CH2:51][CH3:52])[CH3:49]>O1CCCC1>[OH:18][C:19]([CH3:24])([CH3:23])[C:20]([N:50]1[CH2:51][CH2:52][N:7]([C:8]([O:10][CH2:11][C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)=[O:9])[CH2:49][CH2:48]1)=[O:21]

参加物

7

反応物 5

HCID 8471TriethylamineHCID 116712-Hydroxyisobutyric acidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 69316859HCID 69316859、化合物

生成物 1

HCID 21949151HCID 21949151、化合物収率 92.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Benzyl piperazine-1-carbamate (2.203 g, 10.0 mmol) was dissolved in tetrahydrofuran (50 ml); 2-hydroxy-2-methylpropionic acid (1.25 g, 12.0 mmol), 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (2.30 g, 12.0 mmol), 1-hydroxy-1H-benzotriazole monohydrate (1.84 g, 12.0 mmol) and triethylamine (3.35 ml, 24.0 mmol) were added; and the reaction mixture was stirred at room temperature for 7 hours. The reaction mixture was partitioned between ethyl acetate and 1N hydrochloric acid. The organic layer was washed with water, a saturated aqueous solution of sodium hydrogencarbonate and brine, and dried over anhydrous sodium sulfate. The solvent was distilled off, and dried under reduced pressure to yield the title compound (2.823 g, 9.21 mmol, 92.1%) as a colorless oil.

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and 1N hydrochloric acid
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and brine, and dried over anhydrous sodium sulfate
  4. distillationThe solvent was distilled off
  5. customdried under reduced pressure

出典と根拠

ORDレコード
ord-3255af95b5c14c1c8c43d28e9eb4530c
出典データセット
uspto-grants-2008_12
特許番号
US07468380B2

反応ノート

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