Triisopropyl phosphite → HCID 178478281, 화합물

HRID 75211

반응식

HRID 75211 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-ea4693b008a44de7891260c6aeea6471
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835423B2

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