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Triethylamine → HCID 57791769、化合物

HRID 1091722
ノート
印刷プレビュー

反応式

HRID 1091722 の反応式
C(N(CC)CC)C.[O:8]=[C:9]1[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[C:12]([CH2:19][C:20]2[CH:25]=[CH:24][N:23]=[C:22]([C:26]([OH:28])=O)[CH:21]=2)=[N:11][NH:10]1.Cl.[CH:30]1([O:35][CH:36]2[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]2)[CH2:34][CH2:33][CH2:32][CH2:31]1.F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1>CC(N(C)C)=O>[CH:30]1([O:35][CH:36]2[CH2:41][CH2:40][N:39]([C:26]([C:22]3[CH:21]=[C:20]([CH2:19][C:12]4[C:13]5[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=5)[C:9](=[O:8])[NH:10][N:11]=4)[CH:25]=[CH:24][N:23]=3)=[O:28])[CH2:38][CH2:37]2)[CH2:34][CH2:33][CH2:32][CH2:31]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 470028554-(cyclopentyloxy)piperidine hydrochlorideHCID 59767737HCID 59767737、化合物

生成物 1

HCID 57791769HCID 57791769、化合物収率 8.3%

試薬・触媒・溶媒 1

HCID 31374
Dimethylacetamide
溶媒

反応条件

温度
20 °C

実験手順

Triethylamine (0.452 ml, 3.24 mmol) was added in one portion to 4-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)picolinic acid (5) (304 mg, 1.08 mmol), 4-(cyclopentyloxy)piperidine hydrochloride (183 mg, 1.08 mmol) and O-benzotriazol-1-yl-N,N,N′,N′-tetra-methyluronium hexafluorophosphate (533 mg, 1.41 mmol) in DMA (3 ml) at 20° C. under air. The resulting mixture was stirred at 20° C. for 3 days. The crude product was purified by preparative HPLC (Waters XBridge Prep C18 OBD column, 5μ silica, 19 mm diameter, 100 mm length), using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the desired material as a white solid (39 mg, 8.3% yield); 1H NMR (400.132 MHz, DMSO) δ 1.28-1.74 (11H, m), 1.82-1.88 (1H, m), 3.08-3.14 (1H, m), 3.20-3.27 (1H, m), 3.44-3.49 (1H, m), 3.53-3.59 (1H, m), 3.96-4.05 (2H, m), 4.40 (2H, s), 7.39 (1H, d), 7.49 (1H, s), 7.83-7.96 (3H, m), 8.28 (1H, d), 8.47 (1H, d), 12.60 (1H, s); m/z (LC-MS, ESI+), RT=1.88 (M+H 433.1).

後処理

  1. customThe crude product was purified by preparative HPLC (Waters XBridge Prep C18 OBD column, 5μ silica, 19 mm diameter, 100 mm length)
  2. additionFractions containing the desired compound
  3. customwere evaporated to dryness

出典と根拠

ORDレコード
ord-cb367a03f93f459d9d47aba04d58715c
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08129380B2

反応ノート

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