Citric Acid → HCID 86734022、化合物

HRID 1576775ノート

反応式

HRID 1576775 の反応式
[CH2:1]([O:3][C@H:4]1[CH2:29][C@@:28]2([CH3:30])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:27]2[C:26](=[O:31])[CH2:25][C@@:24]2([CH3:32])[C@H:11]3[CH2:12][CH2:13][C@@H:14]2[C:15](=[O:23])[CH2:16][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[CH2:6][C@@H:5]1[OH:33])[CH3:2].[C:34]([OH:46])(=[O:45])[CH2:35][C:36]([CH2:41][C:42]([OH:44])=[O:43])([C:38]([OH:40])=[O:39])[OH:37]>C(O)C>[C:34]([OH:46])(=[O:45])[CH2:35][C:36]([CH2:41][C:42]([OH:44])=[O:43])([C:38]([OH:40])=[O:39])[OH:37].[CH2:1]([O:3][C@H:4]1[CH2:29][C@@:28]2([CH3:30])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:27]2[C:26](=[O:31])[CH2:25][C@@:24]2([CH3:32])[C@H:11]3[CH2:12][CH2:13][C@@H:14]2[C:15](=[O:23])[CH2:16][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[CH2:6][C@@H:5]1[OH:33])[CH3:2]

参加物

4

反応物 2

HCID 311Citric AcidHCID 86734023HCID 86734023、化合物

生成物 1

HCID 86734022HCID 86734022、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2β-ethoxy-3α-hydroxy-21-morpholino-5α-pregnane-11,20-dione (0.093 g, 0.2 mmole) in ethanol (1 ml) was treated with a 0.1M solution of citric acid (2 ml, 0.2 mmole) at room temperature. The clear solution was immediately evaporated to dryness at room temperature and redissolved in distilled water (ca. 5 ml). The aqueous solution was stored at 0° overnight and then filtered. The solid collected was washed with distilled water (ca. 1 ml) and the washings and filtrate combined. The residue was dissolved in chloroform and evaporated under vacuum to constant weight (0.0016 g). The filtrate and washings were made up to 9.14 ml with distilled water thereby giving a solution of title compound (pH 3.59) at concentration 10 mg/ml with respect to steroid.

後処理

  1. customThe clear solution was immediately evaporated to dryness at room temperature
  2. dissolutionredissolved in distilled water (ca. 5 ml)
  3. filtrationfiltered
  4. customThe solid collected
  5. washwas washed with distilled water (ca. 1 ml)
  6. dissolutionThe residue was dissolved in chloroform
  7. customevaporated under vacuum to constant weight (0.0016 g)

出典と根拠

ORDレコード
ord-c2adaabddf3547158f1260d40af527ca
出典データセット
uspto-grants-1976_09
特許番号
US03983111

反応ノート

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