Sodium borohydride → HCID 15858642、化合物

HRID 1837234ノート

反応式

HRID 1837234 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:16]2=[O:20])[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][NH:26][CH3:27].[BH4-].[Na+]>CO>[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:20])[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][NH:26][CH3:27]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 1587066511beta-Fluoro-3-hydroxy-7alpha-[5-(methylamino)-pentyl]-estra-1,3,5(10)-trien-17-one

生成物 1

HCID 15858642HCID 15858642、化合物収率 61%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

880 mg of 11β-fluoro-3-hydroxy-7α-(5-(methyl-amino)-pentyl)-estra-1,3,5(10)-trien-17-one is dissolved in 15 ml of methanol, mixed in portions with 252 mg of sodium borohydride and stirred for 15 minutes at room temperature. For working-up, the reaction solution is added to saturated common salt solution, extracted several times with methylene chloride, the organic phases are washed with water, dried on magnesium sulfate and concentrated by evaporation in a vacuum. 540 mg of 11β-fluoro-7α-(5-(methyl-amino)-pentyl)-estra-1,3,5(10)-triene-3,17β-diol is obtained as a foam, [α]D=+63° (c=0.5 in chloroform).

後処理

  1. additionthe reaction solution is added to saturated common salt solution
  2. extractionextracted several times with methylene chloride
  3. washthe organic phases are washed with water
  4. customdried on magnesium sulfate
  5. concentrationconcentrated by evaporation in a vacuum

出典と根拠

ORDレコード
ord-d165227c4f6f4cc6a005d655891f9466
出典データセット
uspto-grants-2004_08
特許番号
US06780855B2

反応ノート

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