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Acetic Anhydride → 9-Acetoxy-3,4-diazatricyclo[4,2,1,02,5]nona-3,7-diene

HRID 1981098
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반응식

HRID 1981098 반응식
[OH:1][CH:2]1[CH:8]2[CH:9]=[CH:10][CH:3]1[CH:4]1[CH:7]2[N:6]=[N:5]1.[C:11](OC(=O)C)(=[O:13])[CH3:12].C(N(CC)CC)C>CCOCC>[C:11]([O:1][CH:2]1[CH:8]2[CH:9]=[CH:10][CH:3]1[CH:4]1[CH:7]2[N:6]=[N:5]1)(=[O:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 8471TriethylamineHCID 70539013HCID 70539013, 화합물

생성물 1

HCID 867400289-Acetoxy-3,4-diazatricyclo[4,2,1,02,5]nona-3,7-diene

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

5 parts of 9-hydroxy-3,4-diazatricyclo[4,2,1,02,5 ]nona-3,7-diene, 5 parts of acetic anhydride, 1 part of triethylamine and 100 parts of ether were refluxed for 24 hours, after which the reaction mixture was extracted twice with 50 parts of water, and the organic phase was dried with MgSO4 and evaporated down in a rotary evaporator to give 6.2 parts (95 mole %) of 9-acetoxy-3,4-diazatricyclo[4,2,1,02,5 ]nona-3,7-diene of melting point 58° C.

후처리

  1. extractionafter which the reaction mixture was extracted twice with 50 parts of water
  2. dry with materialthe organic phase was dried with MgSO4
  3. customevaporated down in a rotary evaporator

출처 및 근거

ORD 기록
ord-37b2695f948348a188a8a1879465d1f0
출처 데이터셋
uspto-grants-1985_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04512795

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