Urea, (2,2-diethoxyethyl)- → 21-Chloro-16alpha-(2,2-diethoxyethoxy)-11beta,17-dihydroxypregna-1,4-diene-3,20-dione

HRID 918405ノート

反応式

HRID 918405 の反応式
[CH2:1]([O:3][CH:4]([O:8][CH2:9][CH3:10])[CH:5]=[N+]=[N-])[CH3:2].C(OC(OCC)CNC(N)=O)C.[Cl:23][CH2:24][C:25](=[O:49])[C@:26]1([OH:48])[C@:43]2([CH3:44])[C@H:29]([C@H:30]3[C@H:40]([C@@H:41]([OH:45])[CH2:42]2)[C@:38]2([CH3:39])[C:33](=[CH:34][C:35](=[O:46])[CH:36]=[CH:37]2)[CH2:32][CH2:31]3)[CH2:28][C@H:27]1[OH:47]>CO>[Cl:23][CH2:24][C:25](=[O:49])[C@:26]1([OH:48])[C@:43]2([CH3:44])[C@H:29]([C@H:30]3[C@H:40]([C@@H:41]([OH:45])[CH2:42]2)[C@:38]2([CH3:39])[C:33](=[CH:34][C:35](=[O:46])[CH:36]=[CH:37]2)[CH2:32][CH2:31]3)[CH2:28][C@H:27]1[O:47][CH2:5][CH:4]([O:8][CH2:9][CH3:10])[O:3][CH2:1][CH3:2]

参加物

5

反応物 3

HCID 1713901Urea, (2,2-diethoxyethyl)-HCID 21520892Ethane, 2-diazo-1,1-diethoxy-HCID 8673375321-Chloro-11beta,16alpha,17-trihydroxypregna-1,4-diene-3,20-dione

生成物 1

HCID 8673375221-Chloro-16alpha-(2,2-diethoxyethoxy)-11beta,17-dihydroxypregna-1,4-diene-3,20-dione

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

A solution of 2,2-diethoxy-1-diazoethane (prepared from 0.0935 mole of N-2,2-diethoxyethyl urea by the method of W. Kirmse and M. Buschhoff, Chem. Ber., 100, 1491 (1967)) in 300 ml of 3:2 ether-pentane is diluted with 100 ml of methanol and cooled to 0°C. 21-Chloro-11β,16α,17-trihydroxypregna-1,4-diene-3,20-dione, 16,17-cycloborate is added in portions until nitrogen evolution ceases. The solvent is removed in vacuo to yield the title compound.

後処理

  1. customThe solvent is removed in vacuo

出典と根拠

ORDレコード
ord-2d813c81b2a043a78d6f4aae31eea7e8
出典データセット
uspto-grants-1976_07
特許番号
US03971773

反応ノート

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