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Hydrochloric Acid → HCID 9932381, 화합물

HRID 651342
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HRID 651342 반응식
C[O:2][C:3](=[O:33])[CH2:4][N:5]1[C:9](=[O:10])[C:8]2([CH2:15][CH2:14][N:13]([CH2:16][C:17]3[C:26]4[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=4)[CH:20]=[CH:19][CH:18]=3)[CH2:12][CH2:11]2)[N:7]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[CH2:6]1.[OH-].[Na+].ClCCl.Cl>C(O)C>[C:17]1([CH2:16][N:13]2[CH2:14][CH2:15][C:8]3([N:7]([C:27]4[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=4)[CH2:6][N:5]([CH2:4][C:3]([OH:33])=[O:2])[C:9]3=[O:10])[CH2:11][CH2:12]2)[C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:20]=[CH:19][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 14798Sodium HydroxideHCID 98034758-(1-Naphthalenylmethyl)-4-oxo-1-phenyl-1,3,8-triazaspiro[4.5]decane-3-acetic acid Methyl Ester

생성물 1

HCID 9932381HCID 9932381, 화합물수율 103.8%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

(8-Naphthalen-1-ylmethyl-4-oxo-1-phenyl-1,3,8-triaza-spiro[4.5]dec-3-yl)-acetic acid methyl ester (44.40 g, 0.1 mol, prepared as described above) was dissolved in a mixture of 2 N sodium hydroxide (165 ml, 0.33 mol) and ethanol (500 ml) and stirred at room temperature for 16 h. Dichloromethane (700 ml) was added and pH was adjusted to 5 by the addition of 6 N hydrochloric acid. The organic phase was separated, washed with water (2×200 ml and concentrated to 300 ml in vacuo. Water (300 ml) and dichloromethane (100 ml) were added and the slurry was stirred overnight. The product was collected by filtration, washed successively with water (4×100 ml, dichloromethane (2×50 ml) and acetone (2×50 ml) and dried, affording the title compound as a powder (44.6 g, 97% yield).

후처리

  1. customThe organic phase was separated
  2. washwashed with water (2×200 ml
  3. concentrationconcentrated to 300 ml in vacuo
  4. additionWater (300 ml) and dichloromethane (100 ml) were added
  5. stirringthe slurry was stirred overnight
  6. filtrationThe product was collected by filtration
  7. washwashed successively with water (4×100 ml, dichloromethane (2×50 ml) and acetone (2×50 ml)
  8. customdried

출처 및 근거

ORD 기록
ord-ddebb3758d9f4d178442cc9d09706a6c
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06277991B1

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