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Ethyl chloroformate → HCID 86734757, 화합물

HRID 371725
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HRID 371725 반응식
[C:1]1([CH2:13][C:14]([O-:16])=[O:15])([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.ClC(OCC)=O.[N-:23]=[N+:24]=[N-:25].[Na+]>O.CC(C)=O.C(N(CC)CC)C>[N-:23]=[N+:24]=[N-:25].[C:1]1([CH2:13][C:14]([O-:16])=[O:15])([CH2:8][C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 10928Ethyl chloroformateHCID 33557Sodium AzideHCID 71401111[1-(2-Methoxy-2-oxoethyl)cycloheptyl]acetate

생성물 1

HCID 86734757HCID 86734757, 화합물

시약·촉매·용매 3

HCID 180Acetone용매3회HCID 962Water용매
HCID 8471
Triethylamine
용매

실험 절차

15.9 g. monomethyl 1,1-cycloheptane-diacetate are dissolved in 100 ml. anhydrous acetone and, in a manner analogous to that described in Example 1, first mixed with 8.1 g. triethylamine in 30 ml. acetone, thereafter with 9.8 g. ethyl chloroformate in 30 ml. anhydrous acetone and finally with 6.5 g. sodium azide in 20 ml. water. After the reaction has taken place, the reaction mixture is extracted as in Example 1 and the solution obtained of monomethyl 1,1-cycloheptane-diacetate azide is rearranged in toluene to the isocyanate. The methyl 1-isocyanatomethyl-1-cycloheptane-acetate obtained is boiled for 3 hours under reflux in 20% hydrochloric acid. Upon evaporation in a vacuum, 1-aminomethyl-1-cycloheptane-acetic acid separates out in the form of its hydrochloride, which is recrystallised from methanol/acetone/ethyl acetate; m.p. 69° - 72° C.

후처리

  1. additionfirst mixed with 8.1 g
  2. extractionthe reaction mixture is extracted as in Example 1

출처 및 근거

ORD 기록
ord-8245d8f3c32e49b98d4d57015b1bfce1
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04087544

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