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Triethylamine → 3-{1-[3-(7,7-Dimethyl-1,4,6,7-tetrahydropyrazolo[4,3-c]pyridin-5-carbonyl)-phenyl]-piperidin-4-yl}-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

HRID 74619
ノート
印刷プレビュー

反応式

HRID 74619 の反応式
[O:1]=[C:2]1[N:8]([CH:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:16]=[C:17]([CH:21]=[CH:22][CH:23]=3)[C:18](O)=[O:19])[CH2:11][CH2:10]2)[CH2:7][CH2:6][C:5]2[CH:24]=[CH:25][CH:26]=[CH:27][C:4]=2[NH:3]1.Cl.Cl.[CH3:30][C:31]1([CH3:40])[CH2:36][NH:35][CH2:34][C:33]2[CH:37]=[N:38][NH:39][C:32]1=2.C(N(CC)CC)C.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F>CN(C=O)C.CO>[CH3:30][C:31]1([CH3:40])[CH2:36][N:35]([C:18]([C:17]2[CH:16]=[C:15]([N:12]3[CH2:13][CH2:14][CH:9]([N:8]4[CH2:7][CH2:6][C:5]5[CH:24]=[CH:25][CH:26]=[CH:27][C:4]=5[NH:3][C:2]4=[O:1])[CH2:10][CH2:11]3)[CH:23]=[CH:22][CH:21]=2)=[O:19])[CH2:34][C:33]2[CH:37]=[N:38][NH:39][C:32]1=2
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471TriethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 583866643-[4-(2-Oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-benzoic acidHCID 667221937,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine dihydrochloride

生成物 1

HCID 42613139
3-{1-[3-(7,7-Dimethyl-1,4,6,7-tetrahydropyrazolo[4,3-c]pyridin-5-carbonyl)-phenyl]-piperidin-4-yl}-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

70.0 mg (0.19 mmol) 3-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-benzoic acid, 60 mg (0.27 mmol) 7,7-dimethyl-4,5,6,7-tetrahydro-1H-pyrazolo[4,3-c]pyridine-dihydrochloride, 100 μL (0.71 mmol) triethylamine and 70.0 mg (0.22 mmol) TBTU in 1 mL DMF were stirred overnight at RT. The reaction mixture was combined with 1 mL methanol and 10 mL ice water. The precipitated product was suction filtered, washed with water and diethyl ether and purified by preparative HPLC. The product fractions were combined and evaporated down i. vac.

後処理

  1. filtrationfiltered
  2. washwashed with water and diethyl ether
  3. custompurified by preparative HPLC
  4. customevaporated down i

出典と根拠

ORDレコード
ord-a1bf0e4a026d4d7580d011bc07c0db9c
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829006B2

反応ノート

読み込み中…

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