Hydrochloric Acid → HCID 70574841、化合物

HRID 1680014ノート

反応式

HRID 1680014 の反応式
[ClH:1].[NH2:2][CH:3]([CH:11]1[NH:15][CH:14]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[C:13]2([CH2:30][CH2:29][N:28]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:27][CH2:26]2)[S:12]1)[C:4]([O:6]C(C)(C)C)=[O:5]>[N+](C)([O-])=O>[ClH:1].[ClH:1].[NH2:2][CH:3]([CH:11]1[NH:15][CH:14]([C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[C:13]2([CH2:26][CH2:27][N:28]([C:31]3[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=3)[CH2:29][CH2:30]2)[S:12]1)[C:4]([OH:6])=[O:5]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 23458748HCID 23458748、化合物

生成物 1

HCID 70574841HCID 70574841、化合物収率 95.5%

試薬・触媒・溶媒 1

HCID 6375Nitromethane溶媒

実験手順

A stream of gaseous hydrogen chloride is passed through a suspension of 11 g (0.0206 mole) of tert-butyl alpha-amino-4-benzyloxycarbonyl-8-phenyl-1-thia-3,8-diazaspiro[4.5]decane-2-acetate (obtained in 4.3) in 200 ml of nitromethane. After 1 hour, a clear solution is obtained which is filtered through "Hyflocel" and the filtrate is evaporated to dryness. The residue is taken up in diethyl ether, filtered and washed with diethyl ether. There are obtained 9.4 g of alpha-amino-4-benzyloxycarbonyl-8-phenyl-1-thia-3,8-diazaspiro[4.5]decane-2-acetic acid dihydrochloride. Yield: 95.5%; M.P. 164°-167° C. (decomposition).

後処理

  1. customa clear solution is obtained which
  2. filtrationis filtered through "Hyflocel"
  3. customthe filtrate is evaporated to dryness
  4. filtrationfiltered
  5. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-32495cf419ef4049971c87f55029ec50
出典データセット
uspto-grants-1981_06
特許番号
US04271172

反応ノート

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