tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate → Carbamic acid, N-[2-[(2-amino-5-methoxyphenyl)amino]ethyl]-, 1,1-dimethylethyl ester

HRID 1914921

反応式

HRID 1914921 の反応式
[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=1[N+:19]([O-])=O)([CH3:4])([CH3:3])[CH3:2]>[OH-].[OH-].[Pd+2].O1CCOCC1>[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][CH2:9][NH:10][C:11]1[CH:16]=[C:15]([O:17][CH3:18])[CH:14]=[CH:13][C:12]=1[NH2:19])([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 1

HCID 59345555tert-Butyl (2-((5-methoxy-2-nitrophenyl)amino)ethyl)carbamate

生成物 1

HCID 59345530Carbamic acid, N-[2-[(2-amino-5-methoxyphenyl)amino]ethyl]-, 1,1-dimethylethyl ester

試薬・触媒・溶媒 2

HCID 9942167Palladium hydroxide触媒HCID 312751,4-Dioxane溶媒

実験手順

A 2 L round bottom flask equipped with a stir bar was charged with a suspension of 20% Pd(OH)2 (5 g) and 1,4-dioxane (800 mL). [2-(5-Methoxy-2-nitrophenylamino)-ethyl]-carbamic acid tert-butyl ester (100 g, 0.32 mol) was added to the suspension. The reaction mixture was hydrogenated (balloon) for 48 h (until the starting material had been consumed) followed by the addition of K2CO3 (100 g) was added to the mixture and stirred for an additional 12 h to remove traces of water. The suspension was filtered to remove the Pd(OH)2 and K2CO3. The filtrate was used in the next step without further purification (yield not determined).

後処理

  1. customA 2 L round bottom flask equipped with a stir bar
  2. customfor 48 h
  3. customhad been consumed)
  4. additionfollowed by the addition of K2CO3 (100 g)
  5. additionwas added to the mixture
  6. customto remove traces of water
  7. filtrationThe suspension was filtered
  8. customto remove the Pd(OH)2 and K2CO3
  9. customThe filtrate was used in the next step without further purification (
  10. customyield not

出典と根拠

ORDレコード
ord-0e288ddbedd74940acb2275fc30710e2
出典データセット
uspto-grants-2013_12
特許番号
US08614243B2

関連ノート

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