Isopropylamine → 1-{4-[2-(Allyloxy)-ethyl]phenoxy}-3-isopropylamino propan-2-ol

HRID 1765492ノート

反応式

HRID 1765492 の反応式
[CH2:1]([O:4][CH2:5][CH2:6][C:7]1[CH:17]=[CH:16][C:10]([O:11][CH2:12][CH:13]2[CH2:15][O:14]2)=[CH:9][CH:8]=1)[CH:2]=[CH2:3].[CH:18]([NH2:21])([CH3:20])[CH3:19]>CO>[CH2:1]([O:4][CH2:5][CH2:6][C:7]1[CH:17]=[CH:16][C:10]([O:11][CH2:12][CH:13]([OH:14])[CH2:15][NH:21][CH:18]([CH3:20])[CH3:19])=[CH:9][CH:8]=1)[CH:2]=[CH2:3]

参加物

4

反応物 2

HCID 6363IsopropylamineHCID 167262652-[4-(2-Allyloxy-ethyl)-phenoxymethyl]-oxirane

生成物 1

HCID 116593381-{4-[2-(Allyloxy)-ethyl]phenoxy}-3-isopropylamino propan-2-ol収率 75%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of the compound of formula (5) (3.70 g, 0.016 mol), isopropyl amine (7.46 ml, 0.127 mol) in methanol (20 ml) was stirred under reflux for 2 hours and then concentrated. The residue was partitioned between chloroform and water. The organic layer was dried over anhydrous sodium sulphate, filtered and concentrated. The residue was crystallized from pet ether to afford compound of formula (1) as a white solid 3.47 g (75%) mp 52–53° C.

後処理

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated
  3. customThe residue was partitioned between chloroform and water
  4. dry with materialThe organic layer was dried over anhydrous sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was crystallized from pet ether

出典と根拠

ORDレコード
ord-2f976705f55d4c7eb0570c4bdabb6027
出典データセット
uspto-grants-2007_06
特許番号
US07227039B2

反応ノート

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