HCID 67199810, 화합물 → HCID 86621654, 화합물

HRID 547565노트

반응식

HRID 547565 반응식
[ClH:1].[NH2:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2[CH:15]=[CH:14][C:13]([NH:16]C(=O)C)=[CH:12][CH:11]=2)[CH:6]=[C:5]([CH3:20])[N:4]=1>Cl>[ClH:1].[NH2:16][C:13]1[CH:12]=[CH:11][C:10]([NH:9][C:7]2[CH:6]=[C:5]([CH3:20])[N:4]=[C:3]([NH2:2])[N:8]=2)=[CH:15][CH:14]=1

참가 물질

3

반응물 1

HCID 67199810HCID 67199810, 화합물

생성물 1

HCID 86621654HCID 86621654, 화합물수율 99.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

To a suspension of 16 (6.0 g, 20 mmol) was added 2N HCl (40 mL) and the mixture was refluxed for 20 h. The solvents were evaporated to dryness, residue boiled in MeOH and diluted with EtOAc. The resulting precipitate was filtered and washed with EtOAc and dried to give essentially pure 17 (5.0 g, 97%); mp (MeOH/EtOAc) 275-280° C.; 1H NMR [(CD3)2SO] δ 12.50 (br, 1 H, N+H), 10.75 (br s, 1 H, NH), 9.75 (br s, 2 H, NH2), 7.85 (br s, 4 H, NH2 & ArH)), 7.34 (d, J=8.6 Hz, 2 H, ArH), 6.24 (br s, 1 H, ArH), 2.79 (s, 3 H, CH3), HRMS (FAB+) calc. for C11H14N5 (M+1) m/z 216.1249, found 216.1247.

후처리

  1. temperaturethe mixture was refluxed for 20 h
  2. customThe solvents were evaporated to dryness, residue
  3. additiondiluted with EtOAc
  4. filtrationThe resulting precipitate was filtered
  5. washwashed with EtOAc
  6. customdried

출처 및 근거

ORD 기록
ord-dc63f2df74344b81bdaad353d1faac06
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939546B2

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