Rocuronium Bromide Impurity 31 → Rocuronium Bromide Impurity 51

HRID 329957

反応式

HRID 329957 の反応式
[C:1]([O:4][C@@H:5]1[C@@H:22]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[CH2:21][C@@:20]2([CH3:29])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][C@H:13]([N:34]3[CH2:38][CH2:37][CH2:36][CH2:35]3)[C@@H:14]2[O:30]C(=O)C)[CH2:6]1)(=[O:3])[CH3:2]>CO>[C:1]([O:4][C@@H:5]1[C@@H:22]([N:23]2[CH2:24][CH2:25][O:26][CH2:27][CH2:28]2)[CH2:21][C@@:20]2([CH3:29])[C@@H:7]([CH2:8][CH2:9][C@@H:10]3[C@@H:19]2[CH2:18][CH2:17][C@@:15]2([CH3:16])[C@H:11]3[CH2:12][C@H:13]([N:34]3[CH2:35][CH2:36][CH2:37][CH2:38]3)[C@@H:14]2[OH:30])[CH2:6]1)(=[O:3])[CH3:2]

参加物

3

反応物 1

HCID 54054638Rocuronium Bromide Impurity 31

生成物 1

HCID 18637387Rocuronium Bromide Impurity 51収率 85.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol diacetate (6.0 g) in methanol (70 ml) was set aside at room temperature for 20 h., during which time the product partially crystallised. Water (150 ml) was added to precipitate the product as a yellow solid, which was filtered off and dried. The crude solid was recrystallised from ethanol (110 ml) to give (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol 3-acetate (4.70 g), m.p. 112°-118° C.; [α]D20 =+33.1° (c 0.97 in CHCl3)

後処理

  1. customthe product partially crystallised
  2. additionWater (150 ml) was added
  3. customto precipitate the product as a yellow solid, which
  4. filtrationwas filtered off
  5. customdried
  6. customThe crude solid was recrystallised from ethanol (110 ml)

出典と根拠

ORDレコード
ord-ab2c162a34bf498bb78f99e8c967b79e
出典データセット
uspto-grants-1990_01
特許番号
US04894369

関連ノート

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