Ammonia → BOC-Nva-Met-NH2

HRID 851722ノート

反応式

HRID 851722 の反応式
[NH:1]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C@H:2]([C:6]([NH:8][C@H:9]([C:14](OC)=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5].[NH3:25]>CO>[C:21]([O:20][C:18]([NH:1][C@H:2]([C:6]([NH:8][C@H:9]([C:14]([NH2:25])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5])=[O:19])([CH3:24])([CH3:23])[CH3:22]

参加物

4

反応物 2

HCID 222AmmoniaHCID 57129312BOC-Nva-Met-OMe

生成物 1

HCID 57006973BOC-Nva-Met-NH2

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

1.81 g (5 mmoles) of BOC-Nva-Met-OMe are dissolved in 20 ml of methanol, and gaseous ammonia is introduced into the solution for 0.5 hours under ice cooling. The reaction mixture is allowed to stand at room temperature overnight, and then stored in a cold place for some hours. The separated crystalline product is filtered off to obtain 1.27 g of the desired product. The filtrate is evaporated, and the residue is recrystallized from 5 ml of ethanol to obtain further 0.35 g of the product. Thus 1.62 g (93%) of BOC-Nva-Met-NH2 are obtained; m.p.: 166°-167° C., Rf2 =0.57, [α]D25 =-40.9° (c=1%, in methanol).

後処理

  1. waitstored in a cold place for some hours
  2. filtrationThe separated crystalline product is filtered off

出典と根拠

ORDレコード
ord-1b9055973adf431eb7700a171389b852
出典データセット
uspto-grants-1983_05
特許番号
US04386073

反応ノート

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