Phosgene → HCID 59863032, 화합물

HRID 2064066노트

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HRID 2064066 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1.[C:23](Cl)(Cl)=[O:24].C(N(CC)CC)C>ClCCl>[Cl:8][C:5]1[CH:6]=[CH:7][C:2]2[NH:1][C:23](=[O:24])[N:9]([CH:10]3[CH2:11][CH2:12][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:14][CH2:15]3)[C:3]=2[CH:4]=1

참가 물질

5

반응물 3

HCID 6371PhosgeneHCID 8471TriethylamineHCID 57423910HCID 57423910, 화합물

생성물 1

HCID 59863032HCID 59863032, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

1,1-Dimethylethyl 4-[(2-amino-5-chlorophenyl)amino]-1-piperidinecarboxylate (D28) (5.8 g) was dissolved in 100 ml of dichloromethane at 0° C. and phosgene (20% in toluene, 10 ml) and triethylamine (5.6 ml) were added and the mixture was stirred at 0° C. for 1 h, then washed with aqueous citric acid, dried over MgSO4, filtered and evaporated The product was crystallised from diethyl ether to yield the title compound, 5.7 g.

후처리

  1. washwashed with aqueous citric acid
  2. dry with materialdried over MgSO4
  3. filtrationfiltered
  4. customevaporated The product
  5. customwas crystallised from diethyl ether

출처 및 근거

ORD 기록
ord-78cc5d8a778a4467839a0aed8a6e065e
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288413B2

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