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5-Propyl-2,3,6,7-tetrahydro-1H-azepine-2-carboxylic acid [2-chloro-1-(3,4,5-trihydroxy-6-methylsulfanyl-tetrahydro-pyran-2-yl)-propyl]-amide → 5-Propyl-azepane-2-carboxylic acid [2-chloro-1-(3,4,5-trihydroxy-6-methylsulfanyl-tetrahydro-pyran-2-yl)-propyl]-amide

HRID 1269020
ノート
印刷プレビュー

反応式

HRID 1269020 の反応式
[Cl:1][CH:2]([CH3:28])[CH:3]([NH:15][C:16]([CH:18]1[CH2:24][CH:23]=[C:22]([CH2:25][CH2:26][CH3:27])[CH2:21][CH2:20][NH:19]1)=[O:17])[CH:4]1[CH:9]([OH:10])[CH:8]([OH:11])[CH:7]([OH:12])[CH:6]([S:13][CH3:14])[O:5]1>[Pd].CO>[Cl:1][CH:2]([CH3:28])[CH:3]([NH:15][C:16]([CH:18]1[CH2:24][CH2:23][CH:22]([CH2:25][CH2:26][CH3:27])[CH2:21][CH2:20][NH:19]1)=[O:17])[CH:4]1[CH:9]([OH:10])[CH:8]([OH:11])[CH:7]([OH:12])[CH:6]([S:13][CH3:14])[O:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 724404095-Propyl-2,3,6,7-tetrahydro-1H-azepine-2-carboxylic acid [2-chloro-1-(3,4,5-trihydroxy-6-methylsulfanyl-tetrahydro-pyran-2-yl)-propyl]-amide2 回

生成物 1

HCID 730964105-Propyl-azepane-2-carboxylic acid [2-chloro-1-(3,4,5-trihydroxy-6-methylsulfanyl-tetrahydro-pyran-2-yl)-propyl]-amide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

The unsaturated title compound from example 46 5-Propyl-2,3,6,7-tetrahydro-1H-azepine-2-carboxylic acid [2-chloro-1-(3,4,5-trihydroxy-6-methylsulfanyl-tetrahydro-pyran-2-yl)-propyl]-amide (433 mg, 0.99 mmol) and 10% Pd/C (80 mg), were taken MeOH (10 mL) hydrogenated at 50 psi overnight. The solvent was removed to obtain the crude material. Purification was carried by silica gel column chromatography (20% MeOH/DCM) followed by preparative HPLC (general method AC) to furnish isomer 1 Rt=18.3 min (10 mg, 2.3%) and isomer 2 Rt=18.6 min (58 mg, 13.3%).

後処理

  1. customhydrogenated at 50 psi overnight
  2. customThe solvent was removed

出典と根拠

ORDレコード
ord-2ab253b6e60647f1813b8429d3c1e806
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07199106B2

反応ノート

読み込み中…

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