Trifluoroacetic acid → HCID 67108619, 화합물

HRID 1432956노트

반응식

HRID 1432956 반응식
F[C:2](F)(F)[C:3]([OH:5])=O.C(OC([N:15]1[C:23]2[CH:22]=[CH:21][N:20]=[CH:19][C:18]=2[CH:17]=[C:16]1[CH2:24][N:25]1[C:30](=[O:31])[CH2:29][N:28]([S:32]([CH:35]=[CH:36][C:37]2[S:38][C:39]([Cl:42])=[CH:40][CH:41]=2)(=[O:34])=[O:33])C[CH:26]1CO)=O)(C)(C)C>C(Cl)Cl>[Cl:42][C:39]1[S:38][C:37]([CH:36]=[CH:35][S:32]([N:28]2[CH:2]([CH2:3][OH:5])[CH2:26][N:25]([CH2:24][C:16]3[NH:15][C:23]4[CH:22]=[CH:21][N:20]=[CH:19][C:18]=4[CH:17]=3)[C:30](=[O:31])[CH2:29]2)(=[O:34])=[O:33])=[CH:41][CH:40]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 54519295HCID 54519295, 화합물

생성물 1

HCID 67108619HCID 67108619, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (1.8 mL) is added to a solution of 2-{4-[2-(5-chloro-thiophen-2-yl)-ethenesulfonyl]-2-(±)-hydroxymethyl-6-oxo-piperazin-1-ylmethyl}-pyrrolo[3,2-c]pyridine-1-carboxylic acid tert-butyl ester (0.04 g) in CH2Cl2 (4.2 mL) at RT. The reaction mixture is stirred for 4 h then concentrated in vacuo. The title compound is purified by RP-HPLC eluting in a gradient of 10% CH3CN/H2O (0.1% TFA) to 100% CH3CN and lyophilizing the appropriate product fractions. 1H NMR (DMSO-d6, 300 MHz) δ9.10 (s, 1H), 8.46 (d, 1H), 7.82 (d, 1H), 7.50 (d, 1H) 7.43 (d, 1H), 7.14 (d, 1H), 7.01 (d, 1H), 6.94 (s, 1H), 5.12 (bs, 1H), 4.80 (AB, 2H), 3.98 (d, 2H0, 3.90 (m, 1H), 3.40-3.50 (m, 4H). APCI MS, [M+H]+=467, 469.

후처리

  1. concentrationthen concentrated in vacuo
  2. customThe title compound is purified by RP-HPLC
  3. washeluting in a gradient of 10% CH3CN/H2O (0.1% TFA) to 100% CH3CN

출처 및 근거

ORD 기록
ord-b514ac8644d34422bbb7d06e525b0f7f
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07612075B2

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