Triethylamine → 1-Benzyloxycarbonylamino-3-methoxy-2-propanol

HRID 1729320ノート

反応式

HRID 1729320 の反応式
C(N(CC)CC)C.[NH2:8][CH2:9][CH:10]([OH:14])[CH2:11][O:12][CH3:13].[CH2:15]([O:22][C:23](Cl)=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>O1CCCC1.C(OCC)(=O)C>[CH2:15]([O:22][C:23]([NH:8][CH2:9][CH:10]([OH:14])[CH2:11][O:12][CH3:13])=[O:24])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 1245101-Amino-3-methoxypropan-2-ol

生成物 1

HCID 190124911-Benzyloxycarbonylamino-3-methoxy-2-propanol収率 56.7%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

19.69 g of triethylamine are added to a solution of 10.23 g of 1-amino-3- methoxy-2-propanol in 100 ml of tetrahydrofuran. After the mixture is cooled, a solution of 16.60 g of benzyloxycarbonyl chloride in 50 ml of tetrahydrofuran is added dropwise thereto for 30 minutes. The mixture is stirred at room temperature for one hour. The reaction mixture is diluted with ethyl acetate, washed with water and dried. The residue is purified by silica gel column chromatography [solvent: ethyl acetate - hexane (2:1)]. 13.2 g of 1-benzyloxycarbonylamino-3- methoxy-2-propanol are obtained as colorless oil.

後処理

  1. temperatureAfter the mixture is cooled
  2. washwashed with water
  3. customdried
  4. customThe residue is purified by silica gel column chromatography [solvent: ethyl acetate - hexane (2:1)]

出典と根拠

ORDレコード
ord-7a671331d9fe4131b211b8303ad558e2
出典データセット
uspto-grants-1994_07
特許番号
US05332754

反応ノート

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