Methanesulfonic Acid → HCID 19968402, 화합물

HRID 975834노트

반응식

HRID 975834 반응식
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1>CCOCC>[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].[Cl:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]2[C:18]3([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]3)[NH:17][CH2:16][CH2:15][CH:14]=2)=[CH:9][CH:8]=1

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 10220867HCID 10220867, 화합물

생성물 1

HCID 19968402HCID 19968402, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

A solution of methanesulphonic acid (0.3 g) in ether (15 ml) was added dropwise to a cooled solution of 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene (0.8 g, prepared in a similar manner to that described in Example 14) in ether (25 ml). The resulting solid was collected by filtration, washed with ether and dried in vacuo at ambient temperature to yield 5-(4-chlorophenyl)-1-azaspiro[5.5]undec-4-ene methanesulphonate as a white solid. Yield 1.0 g, mp 226°-231.5° C.

후처리

  1. customprepared in a similar manner to that
  2. filtrationThe resulting solid was collected by filtration
  3. washwashed with ether
  4. customdried in vacuo at ambient temperature

출처 및 근거

ORD 기록
ord-d9b7f9ce48f04b17b2fb4d4107a9b341
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05610161

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