HCID 89939678、化合物 → HCID 68310377、化合物

HRID 922424ノート

反応式

HRID 922424 の反応式
C(OC([NH:11][CH2:12][C:13]#[C:14][C:15]1[CH:16]=[C:17]([CH:23]([N:25]([CH:41]2[CH2:43][CH2:42]2)[C:26]([C@@H:28]2[O:33][CH2:32][CH2:31][N:30]([C:34]([O:36][C:37]([CH3:40])([CH3:39])[CH3:38])=[O:35])[CH2:29]2)=[O:27])[CH3:24])[CH:18]=[CH:19][C:20]=1[O:21][CH3:22])=O)C1C=CC=CC=1>CO.[Pd]>[NH2:11][CH2:12][CH2:13][CH2:14][C:15]1[CH:16]=[C:17]([CH:23]([N:25]([CH:41]2[CH2:43][CH2:42]2)[C:26]([C@@H:28]2[O:33][CH2:32][CH2:31][N:30]([C:34]([O:36][C:37]([CH3:38])([CH3:40])[CH3:39])=[O:35])[CH2:29]2)=[O:27])[CH3:24])[CH:18]=[CH:19][C:20]=1[O:21][CH3:22]

参加物

4

反応物 1

HCID 89939678HCID 89939678、化合物

生成物 1

HCID 68310377HCID 68310377、化合物収率 67.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

to a solution of tert-butyl (2R)-2-{[{1-[3-(3-{[(benzyloxy)carbonyl]amino}prop-1-yn-1-yl)-4-methoxyphenyl]ethyl}(cyclopropyl)amino]carbonyl}morpholin-4-carboxylate (2.82 g) in methanol (25 mL) was added 10% palladium on carbon (282 mg), and the mixture was stirred under hydrogen for 7 hours. An insoluble was filtered off, and then the filtrate was concentrated under reduced pressure, and the resulting residue was purified by NH-silica gel column chromatography (eluent: chloroform→chloroform/methanol=33/1) to give tert-butyl (2R)-2-{[{1-[3-(3-aminopropyl)-4-methoxyphenyl]ethyl}(cyclopropyl)amino]carbonyl}morpholin-4-carboxylate [Ex(295-4)] (1.49 g) as a colorless oil.

後処理

  1. filtrationAn insoluble was filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customthe resulting residue was purified by NH-silica gel column chromatography (eluent: chloroform→chloroform/methanol=33/1)

出典と根拠

ORDレコード
ord-e3f0e156207d43dab627779c8bb83bd1
出典データセット
uspto-grants-2016_03
特許番号
US09278944B2

反応ノート

読み込み中…