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Triethylamine → 1-(2-{(3R,4S)-4-[(2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)amino]-3-hydroxy-1-piperidinyl}ethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one Hydrochloride

HRID 656976
ノート
印刷プレビュー

反応式

HRID 656976 の反応式
[ClH:1].Cl.[NH2:3][C@H:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][N:12]2[C:21]3[C:16](=[N:17][CH:18]=[C:19]([F:22])[CH:20]=3)[CH:15]=[CH:14][C:13]2=[O:23])[CH2:6][C@H:5]1[OH:24].C(N(CC)CC)C.[O:32]1[C:41]2[CH:40]=[C:39]([CH:42]=O)[N:38]=[CH:37][C:36]=2[O:35][CH2:34][CH2:33]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>C(Cl)Cl.CO.C(Cl)(Cl)Cl>[ClH:1].[O:32]1[C:41]2[CH:40]=[C:39]([CH2:42][NH:3][C@H:4]3[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][N:12]4[C:21]5[C:16](=[N:17][CH:18]=[C:19]([F:22])[CH:20]=5)[CH:15]=[CH:14][C:13]4=[O:23])[CH2:6][C@H:5]3[OH:24])[N:38]=[CH:37][C:36]=2[O:35][CH2:34][CH2:33]1
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 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 218736682,3-Dihydro[1,4]dioxino[2,3-c]pyridine-7-carbaldehydeHCID 674986531-{2-[(3R,4S)-4-amino-3-hydroxy-1-piperidinyl]ethyl}-7-fluoro-1,5-naphthyridin-2(1H)-one dihydrochloride

生成物 1

HCID 68993163
1-(2-{(3R,4S)-4-[(2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)amino]-3-hydroxy-1-piperidinyl}ethyl)-7-fluoro-1,5-naphthyridin-2(1H)-one Hydrochloride

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 6212Chloroform溶媒HCID 6344Dichloromethane溶媒

実験手順

1-{2-[(3R,4S)-4-Amino-3-hydroxy-1-piperidinyl]ethyl}-7-fluoro-1,5-naphthyridin-2(1H)-one dihydrochloride (100 mg, 0.2637 mmol) was stirred in 9:1 v:v chloroform:MeOH (5 ml) at rt under argon and triethylamine (129 μl, 3.5 eq.) was added. The mixture was stirred at rt for 10 mins, then 2,3-dihydro[1,4]dioxino[2,3-c]pyridine-7-carboxaldehyde (for a synthesis see WO2004058144, Example 2(c) or WO03/087098, Example 19(d)) (44 mg, 0.264 mmol) was added and the mixture was stirred at rt for 1 h before being treated with sodium triacetoxyborohydride (168 mg) added in one portion. The mixture was then stirred at rt over the weekend. Saturated aqueous sodium hydrogen cabonate (2 ml) was then added and the organic phase was diluted with DCM to bring the total volume to ca. 20 ml. The organic phase was separated using a hydrophobic frit and the aqueous phase was extracted with DCM (2×20 ml). The combined DCM extracts were evaporated under reduced pressure and purified by MDAP to give the free base of the title compound as an off-white foam (66 mg).

後処理

  1. additionwas added
  2. stirringthe mixture was stirred at rt for 1 h
  3. additionadded in one portion
  4. stirringThe mixture was then stirred at rt over the weekend
  5. customThe organic phase was separated
  6. extractionthe aqueous phase was extracted with DCM (2×20 ml)
  7. customThe combined DCM extracts were evaporated under reduced pressure
  8. custompurified by MDAP

出典と根拠

ORDレコード
ord-b3365f43d3d8493da510034b7f310726
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071592B2

反応ノート

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