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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
ノート
印刷プレビュー

反応式

HRID 356162 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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%)

出典と根拠

ORDレコード
ord-1808f9e6f91a4d5e9a91a0c226f17b4c
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05834463

反応ノート

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