2-(2-Diazoethoxy)oxane → 21-Chloro-11beta,17-dihydroxy-16alpha-[2-(tetrahydropyran-2-yloxy)ethoxy]-pregna-1,4-diene-3,20-dione

HRID 918415ノート

反応式

HRID 918415 の反応式
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[O:7][CH2:8][CH:9]=[N+]=[N-].[Cl:12][CH2:13][C:14](=[O:38])[C@:15]1([OH:37])[C@:32]2([CH3:33])[C@H:18]([C@H:19]3[C@H:29]([C@@H:30]([OH:34])[CH2:31]2)[C@:27]2([CH3:28])[C:22](=[CH:23][C:24](=[O:35])[CH:25]=[CH:26]2)[CH2:21][CH2:20]3)[CH2:17][C@H:16]1[OH:36]>CCOCC.CO>[Cl:12][CH2:13][C:14](=[O:38])[C@:15]1([OH:37])[C@:32]2([CH3:33])[C@H:18]([C@H:19]3[C@H:29]([C@@H:30]([OH:34])[CH2:31]2)[C@:27]2([CH3:28])[C:22](=[CH:23][C:24](=[O:35])[CH:25]=[CH:26]2)[CH2:21][CH2:20]3)[CH2:17][C@H:16]1[O:36][CH2:9][CH2:8][O:7][CH:2]1[CH2:3][CH2:4][CH2:5][CH2:6][O:1]1

参加物

5

反応物 2

HCID 215208792-(2-Diazoethoxy)oxaneHCID 8673375321-Chloro-11beta,16alpha,17-trihydroxypregna-1,4-diene-3,20-dione

生成物 1

HCID 2279178221-Chloro-11beta,17-dihydroxy-16alpha-[2-(tetrahydropyran-2-yloxy)ethoxy]-pregna-1,4-diene-3,20-dione

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3283Diethyl Ether溶媒

実験手順

A solution of 2-(tetrahydropyran-2-yloxy)-1-diazoethane (prepared from 0.21 mole of N-[2-(tetrahydropyran-2-yloxy)ethyl]urea as described in Example 1) in 400 ml of 3:1 ether-pentane is diluted with 100 ml each of ether and methanol at 0°C and stirred vigorously while 21-chloro-11β,16α,17-trihydroxypregna-1,4-diene-3,20-dione, 16,17-cycloborate (12 mmoles) is added. After nitrogen evolution ceases the solvents are removed in vacuo to yield the title compound.

後処理

  1. additionis added
  2. customare removed in vacuo

出典と根拠

ORDレコード
ord-9c873323b49c432aba26e9e91a416864
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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