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Hydrazine hydrate (1:1) → (3aR*,10aS*)-4-(Aminoacetyl)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one

HRID 356162
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HRID 356162 반응식
[CH2:1]([N:8]1[C:14](=[O:15])[C@H:13]2[CH2:16][CH2:17][CH2:18][C@H:12]2[N:11]([C:19](=[O:32])[CH2:20][N:21]2C(=O)C3=CC=CC=C3C2=O)[C:10]2[CH:33]=[CH:34][CH:35]=[CH:36][C:9]1=2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.O.NN.ClCCl.C(OC(C)C)(C)C>C(O)C>[NH2:21][CH2:20][C:19]([N:11]1[C@@H:12]2[CH2:18][CH2:17][CH2:16][C@@H:13]2[C:14](=[O:15])[N:8]([CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:9]2[CH:36]=[CH:35][CH:34]=[CH:33][C:10]1=2)=[O:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24654Hydrazine hydrate (1:1)HCID 22238436Dichloromethane diisopropyletherHCID 70113585(3aR*,10aS*)-9-benzyl-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one

생성물 1

HCID 70110459(3aR*,10aS*)-4-(Aminoacetyl)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one수율 80%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

A suspension of (3aR*,10aS*)-9-benzyl-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (9.82 g, 20 mmol) and hydrazine monohydrate (2.31 g, 46 mmol) in ethanol (200 mL) was refluxed for 3.5 hours. The reaction mixture was cooled, which was subjected to filtration. The filtrate was washed with chloroform, which was concentrated under reduced pressure. The concentrate was suspended in chloroform, which was again subjected to filtration. The filtrate was concentrated under reduced pressure. The concentrate was crystallized from dichloromethane-hexane to give 5.62 g (yield 80%). The sample for analytical experiment was prepared by recrystallization from dichloromethane-diisopropylether. m.p. 163°-165° C.

후처리

  1. temperaturewas refluxed for 3.5 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationwhich was subjected to filtration
  4. washThe filtrate was washed with chloroform, which
  5. concentrationwas concentrated under reduced pressure
  6. filtrationwhich was again subjected to filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customThe concentrate was crystallized from dichloromethane-hexane
  9. customto give 5.62 g (yield 80%)

출처 및 근거

ORD 기록
ord-1808f9e6f91a4d5e9a91a0c226f17b4c
출처 데이터셋
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05834463

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