Hydrochloric Acid → 1000210-63-8

HRID 1672370노트

반응식

HRID 1672370 반응식
[NH2:1][CH2:2][CH2:3][S:4]([C:7]1[CH:16]=[C:15]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH:14]=[C:13]2[C:8]=1[CH:9]=[CH:10][N:11]=[CH:12]2)(=[O:6])=[O:5].[ClH:24].C([Cl:28])(=O)C.C(OCC)(=O)C>CO>[ClH:28].[ClH:24].[NH2:1][CH2:2][CH2:3][S:4]([C:7]1[CH:16]=[C:15]([C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH:14]=[C:13]2[C:8]=1[CH:9]=[CH:10][N:11]=[CH:12]2)(=[O:5])=[O:6]

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 6367Acetyl chlorideHCID 8857Ethyl AcetateHCID 236358031000210-64-92회

생성물 1

HCID 236584011000210-63-8수율 90%

시약·촉매·용매 1

HCID 887Methanol용매5회

실험 절차

Slurry 4-[5-(2-Amino-ethanesulfonyl)-isoquinolin-7-yl]-phenol (16.57 g, 50.45 mmol) in methanol (500 mL). Separately, prepare a solution of HCl in methanol by adding acetyl chloride (12.60 mL, 177.05 mmol) to methanol (165 mL). Add the solution of HCl in methanol dropwise at room temperature over 30 min to the slurry of 4-[5-(2-Amino-ethanesulfonyl)-isoquinolin-7-yl]-phenol in methanol. Stir for 30 min, then add ethyl acetate (600 mL) dropwise over 1 hour. Stir for 30 min, then filter the solids and wash with ethyl acetate (2×100 mL). Dry solids in vacuo at 50° C., then further dry in vacuo at room temperature with slow administration of nitrogen to afford the title compound (18.3 g, 90%). Mass spectrum (LCMS) m/z=329.0 (M+H+).

후처리

  1. stirringStir for 30 min
  2. filtrationfilter the solids
  3. washwash with ethyl acetate (2×100 mL)
  4. customDry solids in vacuo at 50° C.
  5. customfurther dry in vacuo at room temperature with slow administration of nitrogen

출처 및 근거

ORD 기록
ord-8ad65a14ecf740f09783b658308b0d1b
출처 데이터셋
uspto-grants-2011_08
특허 번호
US07998977B2

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