Hydrochloric Acid → H-Nva-Met-NH2.HCl

HRID 851723ノート

反応式

HRID 851723 の反応式
[NH:1](C(OC(C)(C)C)=O)[C@H:2]([C:6]([NH:8][C@H:9]([C:14]([NH2:16])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5].[ClH:24]>C(OCC)(=O)C.CCOCC>[NH2:1][C@H:2]([C:6]([NH:8][C@H:9]([C:14]([NH2:16])=[O:15])[CH2:10][CH2:11][S:12][CH3:13])=[O:7])[CH2:3][CH2:4][CH3:5].[ClH:24]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 57006973BOC-Nva-Met-NH2

生成物 1

HCID 88736758H-Nva-Met-NH2.HCl収率 89%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

4.5 g (13 mmoles) of BOC-Nva-Met-NH2 are suspended in 20 ml of ethyl acetate, and 20 ml of a 6 n hydrochloric acid solution in ethyl acetate are added to the suspension. After one hour of standing the reaction mixture is diluted with ether, the separated precipitate is filtered off, and dried in vacuo over anhydrous sodium hydroxide. The resulting 4 g of crude product are recrystallized from a mixture of methanol and ether. 3.28 g (89%) of H-Nva-Met-NH2.HCl are obtained; m.p.: 198°-200° C., Rf5 =0.40, [α]D25 =+10.2° (c=1%, in methanol).

後処理

  1. filtrationthe separated precipitate is filtered off
  2. dry with materialdried in vacuo over anhydrous sodium hydroxide
  3. customThe resulting 4 g of crude product are recrystallized from a mixture of methanol and ether

出典と根拠

ORDレコード
ord-76928549785c412ea2c9bc34b93953ca
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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