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Hydrochloric Acid → 7-(3-pyrrolidin-2-yl-benzoylamino)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester HCl

HRID 1524295
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HRID 1524295 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][C:15]([NH:21][C:22](=[O:41])[C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([CH:29]4[CH2:33][CH2:32][CH2:31][N:30]4C(OC(C)(C)C)=O)[CH:24]=3)=[CH:16][CH:17]=2)[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:42].O1CCOCC1>C(Cl)Cl>[ClH:42].[CH2:1]([O:8][C:9]([N:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][C:15]([NH:21][C:22](=[O:41])[C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([CH:29]4[CH2:33][CH2:32][CH2:31][NH:30]4)[CH:24]=3)=[CH:16][CH:17]=2)[CH2:12]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 666551417-[3-(1-tert-butoxycarbonyl-pyrrolidin-2-yl)-benzoylamino]-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester

생성물 1

HCID 666549657-(3-pyrrolidin-2-yl-benzoylamino)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester HCl

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

To a solution of 7-[3-(1-tert-butoxycarbonyl-pyrrolidin-2-yl)-benzoylamino]-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester (900 mg, 1.62 mmol) in methylene chloride (50 mL) add 4M HCl in dioxane (8.1 mL, (32.4 mmol)) and stir the reaction at room temperature for 24 h. Remove the solvents in vacuo at 40° C., dissolve the residue in EtOAc, and concentrate again concentrate to dryness. Dry the residue in vacuo then triturate in EtOAc and hexane to afford 2.63 g of 7-(3-pyrrolidin-2-yl-benzoylamino)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester HCl as a solid.

후처리

  1. customthe reaction at room temperature for 24 h
  2. customRemove the solvents in vacuo at 40° C.
  3. dissolutiondissolve the residue in EtOAc
  4. concentrationconcentrate again
  5. concentrationconcentrate to dryness
  6. customDry the residue in vacuo
  7. customthen triturate in EtOAc

출처 및 근거

ORD 기록
ord-b11f4a532fb54362ba0b126b741d2273
출처 데이터셋
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09079880B2

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