Dimethylformamide → HCID 86656617, 화합물

HRID 2036881노트

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HRID 2036881 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[C:16]([C:21]([OH:23])=O)[CH:17]=2)[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN(C=O)C.C1C=CC2[N:37]([OH:38])N=NC=2C=1.[O:39]1[CH2:44][CH2:43][CH2:42][CH2:41][CH:40]1NO>ClCCl.O.C(Cl)CCl.C(N(CC)CC)C>[O:39]1[CH2:44][CH2:43][CH2:42][CH2:41][CH:40]1[O:38][NH:37][C:21]([C:16]1[CH:17]=[C:18]2[C:13](=[CH:14][CH:15]=1)[CH2:12][N:11]([C:9]([O:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:10])[CH2:20][CH2:19]2)=[O:23]

참가 물질

9

반응물 4

HCID 6228DimethylformamideHCID 757711-HydroxybenzotriazoleHCID 13168123Tetrahydropyranyl hydroxylamineHCID 58399186HCID 58399186, 화합물

생성물 1

HCID 86656617HCID 86656617, 화합물수율 96.6%

시약·촉매·용매 4

HCID 111,2-Dichloroethane용매HCID 962Water용매HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

A mixture of 8.7 g 2-[(benzyloxy)carbonyl]-1,2,3,4-tetrahydroisoquinoline-6-carboxylic acid, 94 ml DMF, 35 ml triethylamine, 4.1 g HOBt and 17 g EDC is stirred for 30 min at ambient temperature. 3.3 g of tetrahydropyran-2-yl-hydroxylamine are added and the reaction mixture is stirred overnight. The mixture is added to a mixture of 100 ml water and 200 ml dichloromethane. The organic phase is separated, washed, dried and evaporated. The crude product is purified by silica gel flash chromatography. 11.08 g of the title compound are obtained as colorless oil.

후처리

  1. stirringthe reaction mixture is stirred overnight
  2. customThe organic phase is separated
  3. washwashed
  4. customdried
  5. customevaporated
  6. customThe crude product is purified by silica gel flash chromatography

출처 및 근거

ORD 기록
ord-bb057419571a4108a392c9c8eb4ba742
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08575193B2

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