Ammonium Chloride → 4-(2-Amino-6-phenoxy-quinolin-3-yl)-N-cyclohexyl-N-methyl-4-(tetrahydro-pyran-4-yl)-butyramide

HRID 252443ノート

反応式

HRID 252443 の反応式
[CH:1]1([N:7]([CH3:39])[C:8](=[O:38])[CH2:9][CH2:10][CH:11]([CH:32]2[CH2:37][CH2:36][O:35][CH2:34][CH2:33]2)[C:12]([C:30]#[N:31])=[CH:13][C:14]2[CH:19]=[C:18]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:17]=[CH:16][C:15]=2[N+:27]([O-])=O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[NH4+].[Cl-]>CO.[Zn]>[NH2:31][C:30]1[C:12]([CH:11]([CH:32]2[CH2:37][CH2:36][O:35][CH2:34][CH2:33]2)[CH2:10][CH2:9][C:8]([N:7]([CH:1]2[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]2)[CH3:39])=[O:38])=[CH:13][C:14]2[C:15](=[CH:16][CH:17]=[C:18]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH:19]=2)[N:27]=1

参加物

5

反応物 2

HCID 25517Ammonium ChlorideHCID 672693405-Cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid cyclohexyl-methyl-amide

生成物 1

HCID 574062904-(2-Amino-6-phenoxy-quinolin-3-yl)-N-cyclohexyl-N-methyl-4-(tetrahydro-pyran-4-yl)-butyramide

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 887Methanol溶媒

実験手順

A solution of 5-cyano-6-(2-nitro-5-phenoxy-phenyl)-4-(tetrahydro-pyran-4-yl)-hex-5-enoic acid cyclohexyl-methyl-amide (0.37 g, 0.697 mmol) in methanol was divided evenly into two microwave tubes containing Zn (0.9 g, 13.8 mmol) and NH4Cl (0.1 g, 1.87 mmol). The reaction mixture was subjected to μW at 95° C. for 900 sec. The reaction mixture was filtered through Celite®, and the filtrate was evaporated in vacuo to yield a crude product which was purified on a silica gel column (10% MeOH/dichloromethane) to yield the title compound as a residue.

後処理

  1. filtrationThe reaction mixture was filtered through Celite®
  2. customthe filtrate was evaporated in vacuo
  3. customto yield a crude product which
  4. customwas purified on a silica gel column (10% MeOH/dichloromethane)

出典と根拠

ORDレコード
ord-15b710a277704cb0b878bec03de5744e
出典データセット
uspto-grants-2011_01
特許番号
US07868022B2

反応ノート

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