反応式
[CH3:1][C:2]1([CH3:18])[CH2:11][CH2:10][C:9]([CH3:13])([CH3:12])[C:8]2[CH:7]=[C:6]([C:14]([NH:16][NH2:17])=[O:15])[CH:5]=[CH:4][C:3]1=2.[C:19]([N:26]1[CH2:31][CH2:30]N(C(O)=O)[CH2:28][CH2:27]1)([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20].Cl.CN(C)CCCN=C=NCC.O.ON1C2C=CC=CC=2N=N1.CN1CC[O:62][CH2:61][CH2:60]1>CN(C=O)C.O>[C:22]([O:21][C:19]([N:26]1[CH2:27][CH2:28][CH:60]([C:61]([NH:17][NH:16][C:14]([C:6]2[CH:5]=[CH:4][C:3]3[C:2]([CH3:18])([CH3:1])[CH2:11][CH2:10][C:9]([CH3:12])([CH3:13])[C:8]=3[CH:7]=2)=[O:15])=[O:62])[CH2:30][CH2:31]1)=[O:20])([CH3:23])([CH3:24])[CH3:25]参加物
反応物 5
HCID 79724-Methylmorpholine
HCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride
HCID 27960291-Hydroxybenzotriazole hydrate
HCID 190015635,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carbohydrazide
HCID 219560274-(Tert-butoxycarbonyl)piperazine-1-carboxylic acid生成物 1
試薬・触媒・溶媒 2
実験手順
2.2 g (6.22 mmol) of 5,5,8,8-tetramethyl-5,6,7,8-tetrahydronaphthalene-2-carboxylic acid hydrazide from step b were suspended in 15 ml of DMF together with 1.43 g (6.22 mmol) of 1-Boc-piperazine-4-carboxylic acid (preparation analogous to Bioorganic & Medicinal Chemistry Letters, 2001, vol. 11, #24 p. 3161-3164), 2.41 g (12.45 mmol) of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride and 867 mg (6.22 mmol) of 1-hydroxybenzotriazole hydrate. 1.40 ml (12.45 mmol) of 4-methylmorpholine were added to the reaction mixture, which was then stirred at room temperature overnight, stirred into 350 ml of water. The resultant precipitate was filtered off with suction, dissolved in DCM, dried, stripped off to dryness and purified by means of flash chromatography on silica gel.
後処理
- filtrationThe resultant precipitate was filtered off with suction
- dissolutiondissolved in DCM
- customdried
- custompurified by means of flash chromatography on silica gel
出典と根拠
- ORDレコード
- ord-3aa2aad101ef4d2a87f114ba358e0575
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08907098B2
関連ノート
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