Methanol → HCID 178453983, 화합물

HRID 1848896노트

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HRID 1848896 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 178453983HCID 178453983, 화합물

시약·촉매·용매 1

HCID 11026Titanium isopropoxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9132d43f0e78493fa0b460b1d569b526
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08952157B2

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