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Chloroform → HCID 12412205, 화합물

HRID 1730260
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HRID 1730260 반응식
[CH:1]1[C:11]2[CH:10]=[CH:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[Cl-:16].[CH2:17]([N+](C1C=CC=CC=1)(C)C)C1C=CC=CC=1.[CH:33]([Cl:36])(Cl)Cl.[OH-:37].[Na+]>O>[Cl:16][C:33]1([Cl:36])[CH:9]2[CH:10]1[C:11]1[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=1[N:6]([CH:17]=[O:37])[C:7]1[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 9212Dibenz(b,f)azepineHCID 14798Sodium Hydroxide2회HCID 76668Benzenemethanaminium, N,N-dimethyl-N-phenyl-, chloride (1:1)

생성물 1

HCID 12412205HCID 12412205, 화합물수율 77.5%

시약·촉매·용매 1

HCID 962Water
용매

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온도
40 °C

실험 절차

At 40° C, 14.48 g. (0.075 mole) of 5H-dibenz(b,f)azepine, 0.57 g. (0.0023 mole) of benzylphenyldimethylammonium chloride, 538 g. (4.5 moles)of chloroform and 360 g. of a 33 % aqueous solution of sodium hydroxide (3.0 moles) are stirred together for 6 hours, after which time 216 g. (5.4moles) of solid sodium hydroxide and 60 g. of water are added. The mixture is stirred at 40° C for 16 hours and the resulting solution is extracted with chloroform. The chloroform extract is washed with water anddried with anhydrous sodium sulfate, followed by distillation of the solvent to dry up under reduced pressure. The residue is then recrystallized from benzene to give 1,1-dichloro-1a,10b-dihydrodibenzo(b,f)cycloprop(d)azepine-6(1H)-carboxaldehyde in a yield of 77.5 % (17.67 g.). Melting point 213° C(decomp.)

후처리

  1. customAt 40° C
  2. extractionthe resulting solution is extracted with chloroform
  3. extractionThe chloroform extract
  4. washis washed with water
  5. distillationfollowed by distillation of the solvent
  6. customto dry up under reduced pressure
  7. customThe residue is then recrystallized from benzene

출처 및 근거

ORD 기록
ord-b630db64efbc450984e8e6e3489dd3cf
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03992370

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