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N-Methylbutylamine → Methyl 5-[(N-methyl-N-butylamino)carbonyl]-2,4-bisbenzyloxybenzoate

HRID 1927697
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HRID 1927697 반응식
[CH2:1]([O:8][C:9]1[CH:18]=[C:17]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:16](Br)=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C]=[O:29].[CH2:30]([N:32]([CH2:35]C)[CH2:33][CH3:34])C.CNCC[CH2:41][CH3:42]>C1COCC1>[CH3:35][N:32]([C:30]([C:16]1[C:17]([O:19][CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[CH:18][C:9]([O:8][CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)=[C:10]([CH:15]=1)[C:11]([O:13][CH3:14])=[O:12])=[O:29])[CH2:33][CH2:34][CH2:41][CH3:42]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8068N-MethylbutylamineHCID 8471TriethylamineHCID 59317108Methyl 5-bromo-2,4-dibenzyloxybenzoateHCID 178418416HCID 178418416, 화합물

생성물 1

HCID 59614016Methyl 5-[(N-methyl-N-butylamino)carbonyl]-2,4-bisbenzyloxybenzoate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

a solution of 55.3 g (129.4 mmol) of methyl 2,4-bisbenzyloxy-5-bromobenzoate, 2.1 g (2.6 mmol) of (1,1′-bis(diphenylphosphino)ferrocene)palladium(11) chloride, 2.9 l of carbon monoxide, 17.7 g (101.2 mmol) of triethylamine, 13.8 g (155.2 mmol) of N-methylbutylamine in 1 l of THF is treated in an autoclave for 20 h at 120° C. and 5-10 bar. The resultant solution is subsequently evaporated and crystallised from ethanol. 59 g (98%) of methyl 5-[(N-methyl-N-butylamino)carbonyl]-2,4-bisbenzyloxybenzoate; MW 461.6.

후처리

  1. customThe resultant solution is subsequently evaporated
  2. customcrystallised from ethanol

출처 및 근거

ORD 기록
ord-3de13dd19c9941caa321faadd5708187
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183279B2

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