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2-Methoxyethanol → [2-Amino-6-(2-methoxy-ethoxy)-3-nitro-pyridin-4-yl]-benzyl-carbamic acid ethyl ester

HRID 639684
ノート
印刷プレビュー

反応式

HRID 639684 の反応式
[H-].[Na+].[CH3:3][O:4][CH2:5][CH2:6][OH:7].[CH2:8]([O:10][C:11](=[O:31])[N:12]([C:20]1[CH:25]=[C:24](Cl)[N:23]=[C:22]([NH2:27])[C:21]=1[N+:28]([O-:30])=[O:29])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:9]>C1COCC1>[CH2:8]([O:10][C:11](=[O:31])[N:12]([C:20]1[CH:25]=[C:24]([O:7][CH2:6][CH2:5][O:4][CH3:3])[N:23]=[C:22]([NH2:27])[C:21]=1[N+:28]([O-:30])=[O:29])[CH2:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[CH3:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 80192-MethoxyethanolHCID 24758Sodium hydrideHCID 57856589(2-Amino-6-chloro-3-nitro-pyridin-4-yl)-benzyl-carbamic acid ethyl ester

生成物 1

HCID 67456853[2-Amino-6-(2-methoxy-ethoxy)-3-nitro-pyridin-4-yl]-benzyl-carbamic acid ethyl ester

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Sodium hydride (21 mg) was added portion-wise to 2-methoxyethanol (0.5 ml). The resultant solution was added drop-wise to a solution of (2-amino-6-chloro-3-nitro-pyridin-4-yl)-benzyl-carbamic acid ethyl ester (100 mg) in THF (1.0 ml). The reaction mixture changed from yellow to deep red/orange solution and was left to stir at RT for 1 h. The orange mixture was concentrated in vacuo then partitioned between EtOAc (10 ml) and saturated NH4Cl solution (10 ml). The layers were separated and the organics were washed with water (10 ml) and brine (10 ml) then dried (MgSO4) and evaporated to provide the title compound as a crude yellow gum (111 mg). This was used directly in the next step with no further purification.

後処理

  1. waitwas left
  2. concentrationThe orange mixture was concentrated in vacuo
  3. customthen partitioned between EtOAc (10 ml) and saturated NH4Cl solution (10 ml)
  4. customThe layers were separated
  5. washthe organics were washed with water (10 ml) and brine (10 ml)
  6. dry with materialthen dried (MgSO4)
  7. customevaporated

出典と根拠

ORDレコード
ord-fa8240b9d4c045d4987c25641a4d1931
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691877B2

反応ノート

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