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 1914921노트

반응식

HRID 1914921 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 9942167Palladium hydroxide촉매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-0e288ddbedd74940acb2275fc30710e2
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08614243B2

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