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Ammonia → HCID 23318048、化合物

HRID 1981895
ノート
印刷プレビュー

反応式

HRID 1981895 の反応式
[C:1]([O:5][C:6]([NH:8][CH:9]([C:28]([OH:30])=[O:29])[CH2:10][CH2:11][S:12][CH2:13][CH:14]([NH2:27])C(C(OCC1C=CC=CC=1)=O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].[Na].N>>[C:1]([O:5][C:6]([NH:8][CH:9]([C:28]([OH:30])=[O:29])[CH2:10][CH2:11][S:12][CH2:13][CH2:14][NH2:27])=[O:7])([CH3:4])([CH3:2])[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 222AmmoniaHCID 5360545SodiumHCID 131714713HCID 131714713、化合物

生成物 1

HCID 23318048HCID 23318048、化合物

実験手順

N-t-Butoxycarbonyl-S-(2-carbobenzyloxycarbonyl aminoethyl)-D,L-homocysteine (1.0 g) is treated with sodium in liquid ammonia according to the procedure described in Example 2. After the ammonia has evaporated off, the residue is extracted with ethanol. Inorganic salts (0.4 g) is removed by filtration. After removal of ethanol, the residue is taken up in 5 ml of water. The aqueous solution is extracted with ether, and then acidified to pH 4 with 4M hydrochloric acid. The solution is concentrated to a volume of 2 ml. Excess ether is added. The product crystallizes out as a white solid (0.32 g). The NMR spectrum (in MeOH-d4 and NaOD) shows a triplet at 3.7, complex absorption between 2.1 and 2.6, a multiplet between 1.5 and 1.9, and a singlet at 1.2.

後処理

  1. customAfter the ammonia has evaporated off
  2. extractionthe residue is extracted with ethanol
  3. customInorganic salts (0.4 g) is removed by filtration
  4. customAfter removal of ethanol
  5. extractionThe aqueous solution is extracted with ether
  6. concentrationThe solution is concentrated to a volume of 2 ml
  7. additionExcess ether is added
  8. customThe product crystallizes out as a white solid (0.32 g)
  9. customat 3.7, complex absorption between 2.1 and 2.6

出典と根拠

ORDレコード
ord-81b6d9fd78824384b5b4e0fc5a019977
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04594341

反応ノート

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