Triisopropyl phosphite → HCID 178478281, 화합물

HRID 1043463

반응식

HRID 1043463 반응식
[Cl:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6]([Cl:27])[C:7]=1[C:8]1[N:9](O)[C:10]2[C:16]3[CH:17]=[N:18][CH:19]=[CH:20][C:15]=3[NH:14][C:13]3[N:21]=[CH:22][CH:23]=[CH:24][C:12]=3[C:11]=2[N:25]=1.P(OC(C)C)(OC(C)C)OC(C)C>CN(C)C(=O)C.C(#N)C.O>[Cl:27][C:6]1[CH:5]=[N:4][CH:3]=[C:2]([Cl:1])[C:7]=1[C:8]1[NH:9][C:10]2[C:16]3[CH:17]=[N:18][CH:19]=[CH:20][C:15]=3[NH:14][C:13]3[N:21]=[CH:22][CH:23]=[CH:24][C:12]=3[C:11]=2[N:25]=1

참가 물질

6

반응물 2

HCID 8304Triisopropyl phosphiteHCID 668869862-(3,5-dichloropyridin-4-yl)imidazo[4,5-d]dipyrido[2,3-b:3',4'-f]azepin-3(8H)-ol

생성물 1

HCID 178478281HCID 178478281, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 31374Dimethylacetamide용매

실험 절차

The crude product from above, 2-(3,5-dichloropyridin-4-yl)imidazo[4,5-d]dipyrido[2,3-b:3′,4′-f]azepin-3(8H)-ol, (0.416 mmol, Intermediate D-8) was dissolved in N,N-dimethylacetamide (1.50 mL) and triisopropyl phosphite (0.19 mL, 0.83 mmol) and heated to 160° C. for 1 h. The mixture was cooled to room temperature, then diluted with acetonitrile and water and the product isolated by preparative HPLC. The pure fractions were combined, concentrated, and then lyophilized to provide the desired product as a yellow powder. 1H NMR (DMSO-d6, 2 tautomers) δ 13.01 (bs, 1H), 8.84 (s, 2H), 8.65 and 8.52 (bs, 1H), 8.42 and 8.15 (bs, 1H), 7.98 (m, 1H), 7.87 (m, 1H), 7.75 and 7.44 (d, 1H), 6.81 (m, 2H). LC/MS: 381, 383 (M+H)+.

후처리

  1. customthe product isolated by preparative HPLC
  2. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c959c662d2b1409cb5202e66fb0eb47b
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08563541B2

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