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Benzyl Alcohol → Benzyl tetrazole-1-acetate

HRID 1733678
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HRID 1733678 반응식
[N:1]1([CH2:6][C:7]([OH:9])=[O:8])[CH:5]=[N:4][N:3]=[N:2]1.[CH2:10](O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.N1C=CC=CC=1.ClC1C=CC(S(ON2C3C=C(Cl)C=CC=3N=N2)(=O)=O)=CC=1>C(C)#N.C(OCC)(=O)C.O>[N:1]1([CH2:6][C:7]([O:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:8])[CH:5]=[N:4][N:3]=[N:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 244Benzyl AlcoholHCID 1049PyridineHCID 5432071-Tetrazolylacetic acidHCID 122228411-(p-Chlorobenzenesulfonyloxy)-6-chloro-1,2,3-benzotriazole

생성물 1

HCID 12222850Benzyl tetrazole-1-acetate수율 74.8%

시약·촉매·용매 3

HCID 962Water용매
HCID 6342Acetonitrile용매
HCID 8857Ethyl Acetate용매

실험 절차

Tetrazole-1-acetic acid (0.64 g), benzyl alcohol (0.65 g) and pyridine (0.80 ml) are dissolved in dry cyanomethane (10 ml) and thereto is added 1-(p-chlorobenzenesulfonyloxy)-6-chloro-1,2,3-benzotriazole (1.72 g) under ice-cooling. After allowing to stand overnight, to the mixture are added water and ethyl acetate. The ethyl acetate layer is washed, dried and concentrated. The precipitated crystals are washed well with ether-petroleum ether to give benzyl tetrazole-1-acetate (815 mg), melting point: 69°-72° C.

후처리

  1. temperaturecooling
  2. washThe ethyl acetate layer is washed
  3. customdried
  4. concentrationconcentrated
  5. washThe precipitated crystals are washed well with ether-petroleum ether

출처 및 근거

ORD 기록
ord-e3a6b0afc9324caa9aeace178db71eb7
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04242507

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