Triethylamine → (3-(2-Pyridyldithio)propionyl) (6-aminohexoxvhydroxy-phosphinyl)oxy-N,N,N-trimethylethanaminium hydroxide

HRID 742943

反応式

HRID 742943 の反応式
[OH-].[NH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][O:9][P:10]([OH:19])([O:12][CH:13]([N+:15]([CH3:18])([CH3:17])[CH3:16])[CH3:14])=[O:11].C(N(CC)CC)C.C1C(=O)N(O[C:35]([CH2:37][CH2:38][S:39][S:40][C:41]2[N:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)=[O:36])C(=O)C1>CS(C)=O>[OH-:9].[N:46]1[CH:45]=[CH:44][CH:43]=[CH:42][C:41]=1[S:40][S:39][CH2:38][CH2:37][C:35]([C:13]([O:12][P:10]([O:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][NH2:2])([OH:19])=[O:11])([N+:15]([CH3:17])([CH3:18])[CH3:16])[CH3:14])=[O:36]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 100682N-Succinimidyl 3-(2-pyridyldithio)propionateHCID 88407369HCID 88407369、化合物

生成物 1

HCID 131719547(3-(2-Pyridyldithio)propionyl) (6-aminohexoxvhydroxy-phosphinyl)oxy-N,N,N-trimethylethanaminium hydroxide

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

2-[(6-Aminohexoxyhydroxyphosphinyl)oxy-N,N,N-trimethylethanaminium hydroxide, inner salt (90 mg, 0.28 mmol) was dissolved in dry dimethyl sulphoxide (2 ml). Triethylamine (197 μl, 1.41 mmol) was added, followed by N-succinimidyl 3-(2-pyridyldithio)propionate (88 mg, 0.28 mmol). The mixture was stirred at ambient temperature for eighteen hours. The solvent was evaporated under vacuum at a temperature of 60° C. and re-evaporated from methanol. The residue was chromatographed on silica gel eluting with methanol. The relevant fractions were combined and evaporated to dryness to give 2[N(3-(2 pyridyldithio)propionyl)(6-aminohexoxyhydroxy

後処理

  1. customThe solvent was evaporated under vacuum at a temperature of 60° C.
  2. customre-evaporated from methanol
  3. customThe residue was chromatographed on silica gel eluting with methanol
  4. customevaporated to dryness
  5. customto give 2[N(3-(2 pyridyldithio)propionyl)(6-aminohexoxyhydroxy

出典と根拠

ORDレコード
ord-3a475cbe09e944b69e8e34e4f420c6a0
出典データセット
uspto-grants-1996_09
特許番号
US05556710

関連ノート

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