Water → N-Boc-1-fluoropent-4-EN-2-amine

HRID 354547

反応式

HRID 354547 の反応式
[C:1]([O:5][C:6]([O:8]N=C(C1C=CC=CC=1)C#N)=O)([CH3:4])([CH3:3])[CH3:2].Cl.[F:20][CH2:21][CH:22]([NH2:26])[CH2:23][CH:24]=[CH2:25].C(N(CC)CC)C.O>O1CCCC1>[F:20][CH2:21][CH:22]([NH:26][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:8])[CH2:23][CH:24]=[CH2:25]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 938652-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrileHCID 205083291-Fluoropent-4-EN-2-amine hcl

生成物 1

HCID 20508337N-Boc-1-fluoropent-4-EN-2-amine収率 85%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Tert-Butyloxycarbonyloxyimino-2-phenylacetonitrile (3.35 g, 13.6 mmoles) in dry tetrahydrofuran (40 ml) is slowly added with ice cooling to a stirred mixture of 1-fluoro-2-amino-4-pentene hydrochloride (1.9 g, 13.6 mmoles) and triethylamine (2.78 g, 27.2 mmoles) in tetrahydrofuran (30 ml). After standing overnight at room temperature, water is added, the tetrahydrofuran is removed under reduced pressure, and the residue is extracted twice with ether. After washing with 1 N sodium hydroxide, then with water until neutral, the organic layer is dried and stripped to give 1-fluoro-2-tert-butoxycarbonylamino-4-pentene (2.33 g, 85%) as an oil which is used without further purification.

後処理

  1. customthe tetrahydrofuran is removed under reduced pressure
  2. extractionthe residue is extracted twice with ether
  3. washAfter washing with 1 N sodium hydroxide
  4. dry with materialwith water until neutral, the organic layer is dried

出典と根拠

ORDレコード
ord-328d7ec2d5e34136ba793b896f94ba5d
出典データセット
uspto-grants-1983_03
特許番号
US04375477

関連ノート

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