Cystamine Dihydrochloride → Fluorescein cystamine

HRID 63754

反応式

HRID 63754 の反応式
Cl.Cl.[NH2:3][CH2:4][CH2:5][S:6][S:7][CH2:8][CH2:9][NH2:10].CCN(C(C)C)C(C)C.C1C(=O)N([O:27][C:28]([C:30]2[C:35]([C:36]3[C:46]4[CH:47]=[CH:48][C:49]([OH:51])=[CH:50][C:45]=4[O:44][C:43]4[C:37]=3[CH:38]=[CH:39][C:40]([CH:42]=4)=[O:41])=[CH:34][CH:33]=[CH:32][CH:31]=2)=[O:29])C(=O)C1>CN(C=O)C.C(OCC)(=O)C>[CH:33]1[CH:32]=[CH:31][C:30]([C:28]([OH:29])=[O:27])=[C:35]([C:36]2[C:37]3[CH:38]=[CH:39][C:40]([OH:41])=[CH:42][C:43]=3[O:44][C:45]3[C:46]=2[CH:47]=[CH:48][C:49]([CH:50]=3)=[O:51])[CH:34]=1.[NH2:3][CH2:4][CH2:5][S:6][S:7][CH2:8][CH2:9][NH2:10]

参加物

6

反応物 3

HCID 5941Cystamine DihydrochlorideHCID 81531DiisopropylethylamineHCID 53393465HCID 53393465、化合物

生成物 1

HCID 86691320Fluorescein cystamine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Cystamine dihydrochloride (68 mg, 0.301 mmol) and DIEA (110 μL, 2.1 eq.) were dissolved in DMF (10 mL), followed by addition of NHS-fluorescein, a mixture of 5- and 6-carboxyfluorescein (300 mg, 0.634 mmol) and the resulting reaction mixture was stirred overnight at room temperature. Then it was diluted with ethyl acetate and washed three times with water and one time with brine. The extract was dried over anhydrous sodium sulfate, concentrated under reduced pressure, redissolved in small amount of methanol and ethyl acetate, and then triturated with diethyl ether to obtain 140 mg of fluorescein-cystamine adduct as a bright orange solid.

後処理

  1. customthe resulting reaction mixture
  2. washwashed three times with water and one time with brine
  3. dry with materialThe extract was dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. dissolutionredissolved in small amount of methanol and ethyl acetate
  6. customtriturated with diethyl ether

出典と根拠

ORDレコード
ord-ce9c8c2a793b4da39941669816888f57
出典データセット
uspto-grants-2016_09
特許番号
US09447035B2

関連ノート

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