Triethylamine → Methylprednisolone Aceponate

HRID 279831

반응식

HRID 279831 반응식
[C:1]([O:4][CH2:5][C:6](=[O:40])[C@:7]1([O:35][C:36](=[O:39])[CH2:37][CH3:38])[C@:24]2([CH3:25])[C@H:10]([C@H:11]3[C@H:21]([C@@H:22]([O:26]C(=O)C(F)(F)F)[CH2:23]2)[C@:19]2([CH3:20])[C:14](=[CH:15][C:16](=[O:33])[CH:17]=[CH:18]2)[C@@H:13]([CH3:34])[CH2:12]3)[CH2:9][CH2:8]1)(=[O:3])[CH3:2].C(N(CC)CC)C>CO>[C:1]([O:4][CH2:5][C:6](=[O:40])[C@:7]1([O:35][C:36](=[O:39])[CH2:37][CH3:38])[C@:24]2([CH3:25])[C@H:10]([C@H:11]3[C@H:21]([C@@H:22]([OH:26])[CH2:23]2)[C@:19]2([CH3:20])[C:14](=[CH:15][C:16](=[O:33])[CH:17]=[CH:18]2)[C@@H:13]([CH3:34])[CH2:12]3)[CH2:9][CH2:8]1)(=[O:3])[CH3:2]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 70466885HCID 70466885, 화합물

생성물 1

HCID 63019Methylprednisolone Aceponate수율 79.1%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

3.5 g of 21-acetoxy-6α-methyl-17-propionyloxy-11β-trifluoroacetoxy-1,4-pregnadiene-3,20-dione is stirred in 80 ml of methanol and 4.2 ml of triethylamine for 4 hours at room temperature. The crude product is purified on 600 g of silica gel with a methylene chloride-acetone gradient (0-15% acetone), thus isolating 2.3 g of 21-acetoxy-11β-hydroxy-6α-methyl-17-propionyloxy-1,4-pregnadiene-3,20-dione.

후처리

  1. customThe crude product is purified on 600 g of silica gel with a methylene chloride-acetone gradient (0-15% acetone)

출처 및 근거

ORD 기록
ord-9b7f0fd4dda74cedad7c2476c5fb953e
출처 데이터셋
uspto-grants-1986_05
특허 번호
US04587236

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