Bromomethylcyclopropane → HCID 70360791、化合物

HRID 329959

反応式

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

参加物

実験手順

Cyclopropylmethyl bromide (1.0 ml) was added to a solution of (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1-pyrrolidinyl)-androstane-3,17-diol diacetate (2.0 g) in acetonitrile (20 ml) and the solution was heated under reflux for 14 d. Evaporation of the reaction mixture to dryness under reduced pressure gave a pale brown solid (2.30 g), which was crystallised from dichloro-methanediethyl ether to remove most of the unreacted starting material. Further purification, by chromatography on alumina as described above, gave material, which was dissolved in dichloro-methane and precipitated from the solution with diethyl ether to give 1-[(2β,3α,5α,16β,17β)-3,17-bis(acetyloxy)-2-(4-morpholinyl)-androstan-16-yl]-1-(cyclopropylmethyl) pyrrolidinium bromide, m.p. decomposes above 175° C.; [α]D20 =-11.6° (c 0.66 in CHCl3).

後処理

temperaturethe solution was heated
temperatureunder reflux for 14 d
customEvaporation of the reaction mixture to dryness under reduced pressure

出典と根拠

ORDレコード: ord-4e324a9ce24d4dd88f0782db38f8c2cb
出典データセット: uspto-grants-1990_01
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04894369

反応式

参加物

反応物 2

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

関連ノート