Rocuronium Bromide Impurity 31 → Rocuronium Bromide Impurity 51

HRID 329957

반응식

HRID 329957 반응식
[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]

참가 물질

3

반응물 1

HCID 54054638Rocuronium Bromide Impurity 31

생성물 1

HCID 18637387Rocuronium Bromide Impurity 51수율 85.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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)

후처리

  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)

출처 및 근거

ORD 기록
ord-ab2c162a34bf498bb78f99e8c967b79e
출처 데이터셋
uspto-grants-1990_01
특허 번호
US04894369

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