Trifluoroacetic acid → Trifluoroacetate

HRID 411820ノート

反応式

HRID 411820 の反応式
[Br:1][CH2:2][C:3]([NH:5][CH2:6][CH2:7][NH:8]C(OC(C)(C)C)=O)=[O:4].[C:16]([OH:22])([C:18]([F:21])([F:20])[F:19])=[O:17]>ClCCl>[Br:1][CH2:2][C:3]([NH:5][CH2:6][CH2:7][NH2:8])=[O:4].[F:19][C:18]([F:21])([F:20])[C:16]([O-:22])=[O:17]

参加物

5

反応物 2

HCID 6422Trifluoroacetic acidHCID 13502099tert-Butyl [2-(2-bromoacetamido)ethyl]carbamate

生成物 2

HCID 84468TrifluoroacetateHCID 22027308HCID 22027308、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-bromoacetyl-N′-BOC-ethylenediamine (3) is dissolved in 50% TFA in dichloromethane (5 ml of the solution per mmol of 3) at 20° C. The deprotection is allowed to proceed for 30 min, then the reaction mixture is concentrated on a rotary evaporator and solidifies upon addition of dry ethyl ether. The solid material is filtered off, washed with ether/petroleum ether on filter and dried. The desired N-bromoacetyl-ethylenediamine is obtained in the form of triflouroacetate salt.

後処理

  1. concentrationthe reaction mixture is concentrated on a rotary evaporator
  2. additionsolidifies upon addition of dry ethyl ether
  3. filtrationThe solid material is filtered off
  4. washwashed with ether/petroleum ether
  5. filtrationon filter
  6. customdried

出典と根拠

ORDレコード
ord-7e479315f5cd4b16921dab24c9bd400f
出典データセット
uspto-grants-2003_05
特許番号
US06559280B2

反応ノート

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