2-Bromo-3-methoxypyridine → HCID 23045060、化合物

HRID 2108036ノート

反応式

HRID 2108036 の反応式
Br[C:2]1[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:10][C:11]1[C:16]([Cl:17])=[CH:15][C:14]([CH:18]([CH2:20][N:21]([CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][O:28][CH2:29][C:30]#[CH:31])[OH:19])=[CH:13][C:12]=1[Cl:39]>C(NCC)C.C1COCC1.[Cu]I>[NH2:10][C:11]1[C:12]([Cl:39])=[CH:13][C:14]([CH:18]([CH2:20][N:21]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][O:28][CH2:29][C:30]#[C:31][C:2]2[C:7]([O:8][CH3:9])=[CH:6][CH:5]=[CH:4][N:3]=2)[CH2:32][C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[OH:19])=[CH:15][C:16]=1[Cl:17]

参加物

6

反応物 2

HCID 903642-Bromo-3-methoxypyridineHCID 200628464-Amino-3,5-dichloro-alpha-[[(phenylmethyl)[6-[(2-propynyl)oxy]hexyl]amino]methyl]benzenemethanol

生成物 1

HCID 23045060HCID 23045060、化合物収率 77.7%

試薬・触媒・溶媒 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)触媒HCID 8021Diethylamine溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 2-bromo-3-methoxypyridine (2 g), 4-amino-3,5-dichloro-α-[[(phenylmethyl)[6-[(2-propynyl)oxy]hexyl]amino]methyl]benzenemethanol (5.74 g), BTPC (150 mg), copper (I) iodide (15 mg) in diethylamine (20 ml) and THF (10 ml) was stirred under nitrogen overnight. The solution was concentrated in vacuo to give a brown oil which was purified by FCC eluting with System C (95:5:1) to give the title compound as a brown oil (4.6 g), t.l.c. (System A 80:20:1) Rf 0.6.

後処理

  1. concentrationThe solution was concentrated in vacuo
  2. customto give a brown oil which
  3. customwas purified by FCC
  4. washeluting with System C (95:5:1)

出典と根拠

ORDレコード
ord-77ec110885904cf684a73fe2a1086a4b
出典データセット
uspto-grants-1990_06
特許番号
US04937251

反応ノート

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