Methanesulfonic Acid → HCID 89845238, 화합물

HRID 539904노트

반응식

HRID 539904 반응식
[Cl:1][C:2]1[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([NH:11][C:12]3[N:17]=[C:16]([N:18]4[CH:22]=[C:21]([CH2:23][N:24]5[CH2:27][CH:26]([OH:28])[CH2:25]5)[C:20]([CH3:29])=[N:19]4)[CH:15]=[CH:14][N:13]=3)[CH:9]=2)[N:4]([CH3:30])[CH:3]=1.[CH3:31][S:32](O)(=[O:34])=[O:33]>CO>[CH3:31][S:32]([O:28][CH:26]1[CH2:25][N:24]([CH2:23][C:21]2[C:20]([CH3:29])=[N:19][N:18]([C:16]3[CH:15]=[CH:14][N:13]=[C:12]([NH:11][C:8]4[CH:9]=[C:10]5[C:5](=[CH:6][CH:7]=4)[N:4]([CH3:30])[CH:3]=[C:2]5[Cl:1])[N:17]=3)[CH:22]=2)[CH2:27]1)(=[O:34])=[O:33]

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 71698378HCID 71698378, 화합물2회

생성물 1

HCID 89845238HCID 89845238, 화합물수율 54%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a slurry of 1-((1-(2-(3-chloro-1-methyl-1H-indol-5-ylamino)pyrimidin-4-yl)-3-methyl-1H-pyrazol-4-yl)methyl)azetidin-3-ol, Compound No. 144 (127 mg, 0.3 mmol) in methanol, was added 1 equivalant of methanesulfonic acid at room temperature. After being stirred at room temperature, the resulting solids were collected by filtration, rinsed with cold methanol and then vacuum dried to give 85 mg (54%) of the desired compound 181 as a pale yellow solid. MS (ESI) m/z 424 [M+H]+; 1H NMR (300 MHz, DMSO-d6) δ 9.9 (br s, 1H), 9.98 (s, 1H), 8.66 (s, 1H), 8.53 (d, 1H, J=5.4 Hz), 7.92 (S, 1H), 7.53˜7.51 (m, 3H), 7.19 (d, 1H, J=5.4 Hz), 4.45˜4.50 (m, 1H), 4.32˜4.38 (m, 2H), 4.22˜4.28 (m, 2H), 3.85˜3.91 (m, 2H), 3.79 (s, 3H), 2.36 (s, 3H).

후처리

  1. filtrationthe resulting solids were collected by filtration
  2. washrinsed with cold methanol
  3. customvacuum dried

출처 및 근거

ORD 기록
ord-2aaad86033d04845a51a416e36ab8013
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08871778B2

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