Water → HCID 15858644、化合物

HRID 1838892ノート

反応式

HRID 1838892 の反応式
[F:1][C@H:2]1[CH2:19][C@@:17]2([CH3:18])[C@@H:13]([CH2:14][CH2:15][C@@H:16]2O)[C@H:12]2[C@H:3]1[C:4]1[CH:5]=[CH:6][C:7]([OH:28])=[CH:8][C:9]=1[CH2:10][CH:11]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:26][CH3:27].S(C1C=CC(C)=CC=1)(O[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][C:40]([F:46])([F:45])[C:41]([F:44])([F:43])[F:42])(=O)=O.[OH2:54]>CN(C)C=O>[F:1][C@H:2]1[CH2:19][C@@:17]2([CH3:18])[C@@H:13]([CH2:14][CH2:15][C@@H:16]2[OH:54])[C@H:12]2[C@H:3]1[C:4]1[CH:5]=[CH:6][C:7]([OH:28])=[CH:8][C:9]=1[CH2:10][C@H:11]2[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][N:26]([CH3:27])[CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][C:40]([F:45])([F:46])[C:41]([F:42])([F:43])[F:44]

参加物

5

反応物 3

HCID 962WaterHCID 15858643HCID 15858643、化合物HCID 69935314HCID 69935314、化合物

生成物 1

HCID 15858644HCID 15858644、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 1.77 g of 11β-fluoro-7x-[5-(methylamino)-pentyl]oestra-1,3,5(10)-triene-3,17β-diol in 18 ml of dimethylformamide is stirred at a bath temperature of 80° C. for 1 hour with 1.4 g of 8,8,9,9,9-penta-fluorononyl tosylate. The mixture is then added to water, extracted 3 times with ethyl acetate, washed with water and sodium chloride solution, dried over sodium sulphate, concentrated in vacuo and the residue is chromatographed on silica gel using dichloromethane/methanol. 11β-Fluoro-7α-{5-[methyl(8,8,9,9,9-penta-fluorononyl)amino]pentyl}oestra-1,3,5(10)-triene-3,17β-diol is obtained as crystals of melting point 11° C.

後処理

  1. extractionextracted 3 times with ethyl acetate
  2. washwashed with water and sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated in vacuo
  5. customthe residue is chromatographed on silica gel

出典と根拠

ORDレコード
ord-550cd8fd8733418b8b39f307fb939b52
出典データセット
uspto-grants-2004_01
特許番号
US06677324B1

反応ノート

読み込み中…