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Benzaldehyde → (3aR*,10aS*)-9-[4-(Benzylamino)benzyl]-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one

HRID 361580
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HRID 361580 반응식
[NH2:1][C:2]1[CH:37]=[CH:36][C:5]([CH2:6][N:7]2[C:13](=[O:14])[C@H:12]3[CH2:15][CH2:16][CH2:17][C@H:11]3[N:10]([C:18](=[O:31])[CH2:19][N:20]3[C:24](=[O:25])[C:23]4=[CH:26][CH:27]=[CH:28][CH:29]=[C:22]4[C:21]3=[O:30])[C:9]3[CH:32]=[CH:33][CH:34]=[CH:35][C:8]2=3)=[CH:4][CH:3]=1.[CH:38](=O)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.CC1C(Br)=C(O)C(Br)=CC=1C1(C2C=C(Br)C(O)=C(Br)C=2C)OS(=O)(=O)C2C=CC=CC1=2.C([BH3-])#N.[Na+].Cl.CO>C(Cl)(Cl)Cl.O.CO>[CH2:38]([NH:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][N:7]2[C:13](=[O:14])[C@H:12]3[CH2:15][CH2:16][CH2:17][C@H:11]3[N:10]([C:18](=[O:31])[CH2:19][N:20]3[C:21](=[O:30])[C:22]4=[CH:29][CH:28]=[CH:27][CH:26]=[C:23]4[C:24]3=[O:25])[C:9]3[CH:32]=[CH:33][CH:34]=[CH:35][C:8]2=3)=[CH:36][CH:37]=1)[C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1
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참가 물질

9

반응물 5

HCID 240BenzaldehydeHCID 6451Bromocresol GreenHCID 5003444Sodium cyanoborohydrideHCID 21893726Hydrochloride methanolHCID 54523300(3aR*,10aS*)-9-(4-aminobenzyl)-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][l,4]diazepin-10(1H)-one

생성물 1

HCID 54536426
(3aR*,10aS*)-9-[4-(Benzylamino)benzyl]-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one
수율 70%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6212Chloroform용매

실험 절차

To a suspension of (3aR*,10aS*)-9-(4-aminobenzyl)-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (198 mg, 0.4 mmol) in chloroform (2 mL)-methanol (2 mL) was added benzaldehyde (49 μL, 0.48 mmol) and the mixture was stirred at room temperature for 40 minutes. To the resulting solution was added bromocresol green as well as sodium cyanoborohydride (30 mg, 0.48 mmol). Then, 10% HCl/methanol was added dropwise until the color of the mixture had ceased to change. This reaction mixture was stirred at room temperature for 15 minutes, at the end of which time it was diluted with water and extracted with 3 portions of chloroform. The pooled organic layer was washed with water, dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was crystallized from ethanol to provide 163 mg (Yield 70%) of the title compound. m.p. 178°-182° C.

후처리

  1. stirringThis reaction mixture was stirred at room temperature for 15 minutes, at the end of which time it
  2. extractionextracted with 3 portions of chloroform
  3. washThe pooled organic layer was washed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was crystallized from ethanol

출처 및 근거

ORD 기록
ord-9125524adaf045f4b992bb9ca259d07f
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866567

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