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Hydrochloric Acid → 10-tert-Butoxycarbonylamino-3-(2-methyl-pyrimidin-5-yl)-dec-4-enoic acid ethyl ester

HRID 2120703
ノート
印刷プレビュー

反応式

HRID 2120703 の反応式
[C:1]([O:5][C:6](=[O:24])[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH:13](O)[CH:14]=[CH:15][C:16]1[CH:17]=[N:18][C:19]([CH3:22])=[N:20][CH:21]=1)([CH3:4])([CH3:3])[CH3:2].C(O)(=O)CC.Cl.[C:31](OCC)([O:36]CC)([O:33][CH2:34][CH3:35])[CH3:32]>[Cl-].[Na+].O>[CH2:34]([O:33][C:31](=[O:36])[CH2:32][CH:15]([C:16]1[CH:17]=[N:18][C:19]([CH3:22])=[N:20][CH:21]=1)[CH:14]=[CH:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][NH:7][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:24])[CH3:35]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1032Propionic AcidHCID 66221Triethyl orthoacetateHCID 73687171[6-Hydroxy-8-(2-methyl-pyrimidin-5-yl)-oct-7-enyl]-carbamic acid tert-butyl ester

生成物 1

HCID 6966645410-tert-Butoxycarbonylamino-3-(2-methyl-pyrimidin-5-yl)-dec-4-enoic acid ethyl ester

試薬・触媒・溶媒 1

HCID 57417360
Sodium chloride; water
溶媒

反応条件

温度
150 °C

実験手順

A solution of 24-4 (1.00 g, 2.98 mmol) in triethyl orthoacetate (50 mL) was treated with propionic acid (2.5 mg, 0.034 mmol) and heated to 150 ° C. for 3 h. The reaction mixture was cooled to room temperature and treated with 1 N HCl and brine (75 mL each). The mixture was extracted with two portions of ethyl acetate. The combined organics were washed with brine and dried (Na2SO4). Purification via PCTLC (SiO2, 4 mm, 10% EtOH; 90% CH2Cl2) afforded 24-5 (650 mg).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionThe mixture was extracted with two portions of ethyl acetate
  3. washThe combined organics were washed with brine
  4. dry with materialdried (Na2SO4)
  5. customPurification via PCTLC (SiO2, 4 mm, 10% EtOH; 90% CH2Cl2)

出典と根拠

ORDレコード
ord-046e4c56d8d94d019e327a7167ea600a
出典データセット
uspto-grants-2004_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06693101B2

反応ノート

読み込み中…

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