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Thionyl Chloride → HCID 13689056, 화합물

HRID 364193
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HRID 364193 반응식
Cl.[CH2:2]([N:4]([CH2:29][CH3:30])[CH2:5][CH2:6][N:7]1[C:15]2[CH:14]=[CH:13][C:12]([N+:16]([O-:18])=[O:17])=[C:11]3[S:19][C:20]4[C:25]([O:26][CH3:27])=[CH:24][CH:23]=[C:22]([OH:28])[C:21]=4[C:9]([C:10]=23)=[N:8]1)[CH3:3].Cl[C:32]1C2C(=O)C3C(=C(OC)C=CC=3O)SC=2C([N+]([O-])=O)=CC=1.ClC1C=CC([N+]([O-])=O)=C(SC2C(OC)=CC=C(OC)C=2C(O)=O)C=1.S(Cl)(Cl)=O.[Al+3].[Cl-].[Cl-].[Cl-]>C1(C)C=CC=CC=1>[CH2:29]([N:4]([CH2:2][CH3:3])[CH2:5][CH2:6][N:7]1[C:15]2[CH:14]=[CH:13][C:12]([N+:16]([O-:18])=[O:17])=[C:11]3[S:19][C:20]4[C:25]([O:26][CH3:27])=[CH:24][CH:23]=[C:22]([O:28][CH3:32])[C:21]=4[C:9]([C:10]=23)=[N:8]1)[CH3:30]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 24386Thionyl ChlorideHCID 6451240Aluminum(III) ChlorideHCID 20240171HCID 20240171, 화합물HCID 20240207HCID 20240207, 화합물HCID 178464048HCID 178464048, 화합물

생성물 1

HCID 13689056HCID 13689056, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

Other 10-hydroxy-7-methoxy-, 10-methoxy-7-hydroxy-, and 7,10-dimethoxy-5-nitro-2-(substituted)-2H[1]benzothiopyrano[4,3,2-cd]indazoles can be prepared in the manner of Examples 33 through 35 and 54. One such compound is 2-[2-(diethylamino)-ethyl]-7-methoxy-5-nitro-2H[1]benzothiopyrano[4,3,2-cd]indazol-10-ol, hydrochloride salt, mp 267°-270° C. The latter compound is prepared from 1-chloro-5-methoxy-8-hydroxy-4-nitro-9H-thioxanthen-9-one which in turn is prepared as follows: A suspension of 5.8 g (0.016 mol) of 2-[(5-chloro-2-nitrophenyl)thio]-3,6-dimethoxybenzoic acid, 50 ml of toluene, and 3.8 g (0.032 mol) of thionyl chloride was heated under reflux for two hours, concentrated to dryness in vacuo, and dissolved in 50 ml of nitrobenzene. The solution was treated portionwise with 3.6 g (0.026 mol) of AlCl3, keeping the temperature below 35° C. during the addition. The mixture was stirred for two hours at 70° C., chilled in a refrigerator overnight, and poured into 400 ml of ice-cold H2O. The mixture was extracted four times with CH2Cl2 and the extracts were combined, dried (MgSO4), and concentrated in vacuo to dryness. The residue was triturated successively in petroleum ether and hot MeOH, and recrystallized from DMF to give 1.2 g of product, 272°-273° C.

후처리

  1. customis prepared
  2. temperaturewas heated
  3. temperatureunder reflux for two hours
  4. concentrationconcentrated to dryness in vacuo
  5. dissolutiondissolved in 50 ml of nitrobenzene
  6. customthe temperature below 35° C.
  7. additionduring the addition
  8. temperaturechilled in a refrigerator overnight
  9. extractionThe mixture was extracted four times with CH2Cl2
  10. dry with materialdried (MgSO4)
  11. concentrationconcentrated in vacuo to dryness
  12. customThe residue was triturated successively in petroleum ether
  13. customhot MeOH, and recrystallized from DMF

출처 및 근거

ORD 기록
ord-bdf54473b13e4b3cb2b82521d880a4b6
출처 데이터셋
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04604390

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