Diisopropylethylamine → HCID 86675758, 화합물

HRID 571536노트

반응식

HRID 571536 반응식
[Cl:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=O)=[C:4]([F:12])[CH:3]=1.C(N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.C[N+](C)=C(N(C)C)ON1C2N=CC=CC=2N=N1.[F:46][CH:47]([F:50])[CH2:48][NH2:49]>ClCCCl.ClC(Cl)C>[Cl:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([NH:49][CH2:48][CH:47]([F:50])[F:46])=[O:8])=[C:4]([F:12])[CH:3]=1

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 1362742,2-DifluoroethanamineHCID 27332744-Chloro-2,5-difluorobenzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

생성물 1

HCID 86675758HCID 86675758, 화합물

시약·촉매·용매 2

HCID 111,2-Dichloroethane용매HCID 63651,1-Dichloroethane용매

실험 절차

A solution of 4-chloro-2,5-difluorobenzoic acid (1.28 g, 6.64 mmol), N,N-diisopropylethylamine (3.5 mL, 20 mmol), and N,N,N′,N′-tetramethyl-O-(7-azabenzotriazol-1-yl)uronium hexafluorophosphate (3.07 g, 8.07 mmol) in 1,2-dichloroethane (20 mL) was stirred for 10 min. at room temperature prior to the addition of a solution of 2,2-difluoroethanamine (538 mg, 6.64 mmol) in dichloroethane (2 mL). The resulting solution was stirred for 1 h. at room temperature. LCMS data indicated that the major reaction component was the desired product. The crude reaction mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column with methanol in dichloromethane (0-10%) to afford the desired product. LCMS (M+H)+: m/z=256.0.

출처 및 근거

ORD 기록
ord-6a00512fdd934978984a21c00bca279e
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09023840B2

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