Hydrochloric Acid → HCID 68680492, 화합물

HRID 639282노트

반응식

HRID 639282 반응식
ClC(Cl)(Cl)[C:3]([C:5]1[N:14]2[C:8]([CH2:9][N:10]([C:19](=[O:29])[CH2:20][O:21][C:22]3[CH:27]=[CH:26][C:25]([Cl:28])=[CH:24][CH:23]=3)[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13]2)=[CH:7][CH:6]=1)=[O:4].[OH-:32].[Na+].Cl>CC(C)=O>[Cl:28][C:25]1[CH:26]=[CH:27][C:22]([O:21][CH2:20][C:19]([N:10]2[C:11]3[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=3[CH2:13][N:14]3[C:5]([C:3]([OH:4])=[O:32])=[CH:6][CH:7]=[C:8]3[CH2:9]2)=[O:29])=[CH:23][CH:24]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 160392192,2,2-trichloro-1-{10-[(4-chlorophenoxy)acetyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone

생성물 1

HCID 68680492HCID 68680492, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

To a stirred solution of 2,2,2-trichloro-1-{10-[(4-chlorophenoxy)acetyl]-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-3-yl}ethanone (0.20 mmol) in acetone (1.2 mL) was added 0.15 mL of 2.5 N sodium hydroxide. After stirring for 20 hours the mixture was acidified with 2.0 N hydrochloric acid, extracted into ethyl acetate, washed with brine, and dried over anhydrous sodium sulfate. The solution was then evaporated and the residue purified by trituration with diethylether. The solid (0.066 g, 83%) was collected and dried, m.p. 168° C. MS [(+)ESI, m/z]: 395 [M+H]+ Anal. Calcd for C21H17CIN2O4: C, 63.56; H, 4.32; N, 7.06. Found: C, 63.66; H, 4.48; N, 6.86

후처리

  1. extractionextracted into ethyl acetate
  2. washwashed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solution was then evaporated
  5. customthe residue purified by trituration with diethylether
  6. customThe solid (0.066 g, 83%) was collected
  7. customdried

출처 및 근거

ORD 기록
ord-7812427471d04d7e8cd24475e2c1de2b
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691848B2

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