Methanol → HCID 178453983、化合物

HRID 1848896ノート

反応式

HRID 1848896 の反応式
Cl.Cl.[O:3]1[CH2:8][CH2:7][CH:6]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH2:5][CH2:4]1.O=[C:16]1[CH2:21][CH2:20][CH:19]([NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26])[CH2:18][CH2:17]1.CO.[BH4-].[Na+]>CC(C)[O-].[Ti+4].CC(C)[O-].CC(C)[O-].CC(C)[O-]>[O:3]1[CH2:8][CH2:7][CH:6]([N:9]2[CH2:14][CH2:13][N:12]([C@H:16]3[CH2:17][CH2:18][C@H:19]([NH:22][C:23](=[O:29])[O:24][C:25]([CH3:27])([CH3:26])[CH3:28])[CH2:20][CH2:21]3)[CH2:11][CH2:10]2)[CH2:5][CH2:4]1

参加物

6

反応物 4

HCID 887MethanolHCID 1512535tert-butyl N-(4-oxocyclohexyl)carbamateHCID 4311764Sodium borohydrideHCID 441204811-(Oxan-4-yl)piperazine--hydrogen chloride (1/2)

生成物 1

HCID 178453983HCID 178453983、化合物

試薬・触媒・溶媒 1

HCID 11026Titanium isopropoxide溶媒

実験手順

To a solution of EXAMPLE 336B (1 g) and tert-butyl 4-oxocyclohexylcarbamate (0.877 g) stirred for 24 hours at room temperature in titanium(IV) isopropoxide (2.410 mL), methanol (2 mL) was added followed by careful addition of sodium borohydride (0.311 g). The reaction mixture was quenched with water, extracted with ether, dried and concentrated. The crude product was purified by flash chromotography (silica 80 g, 50%-100% acetone/hexanes) providing the product.

後処理

  1. customThe reaction mixture was quenched with water
  2. extractionextracted with ether
  3. customdried
  4. concentrationconcentrated
  5. customThe crude product was purified by flash chromotography (silica 80 g, 50%-100% acetone/hexanes)
  6. customproviding the product

出典と根拠

ORDレコード
ord-9132d43f0e78493fa0b460b1d569b526
出典データセット
uspto-grants-2015_02
特許番号
US08952157B2

反応ノート

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