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Methanol → HCID 20264017, 화합물

HRID 1856052
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HRID 1856052 반응식
NC(N)=[S:3].CO.Cl.[CH2:8]([O:15][C:16]1[C:17]([CH3:26])=[N:18][CH:19]=[C:20]([CH:24]=[CH2:25])[C:21]=1[CH2:22]Cl)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.[OH-].[Na+]>O>[CH3:26][C:17]1[C:16]([O:15][CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[C:21]([CH2:22][SH:3])[C:20]([CH:24]=[CH2:25])=[CH:19][N:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 202639413-Benzyloxy-4-chloromethyl-2-methyl-5-vinylpyridine hydrochloride

생성물 1

HCID 20264017HCID 20264017, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a well stirred solution of 0.11 mole of thiourea in 250 ml. methanol, under N2 is added 0.1 mole of 3-benzyloxy-4-chloromethyl-2-methyl-5-vinylpyridine hyrochloride. The mixture is refluxed for 1 hour and then cooled. A solution of 0.4 mole of sodium hydroxide in 50 ml. of water is added, and the resulting mixture refluxed for 30 minutes. After concentration in vacuo the reaction mixture is taken up between benzene and water and enough acetic acid added to neutralize the mixture. The organic layer is separated, washed well with water, dried, and concentrated to give 2-methyl-3-benzyloxy-4-mercaptomethyl-5-vinylpyridine.

후처리

  1. temperatureThe mixture is refluxed for 1 hour
  2. temperaturecooled
  3. temperaturethe resulting mixture refluxed for 30 minutes
  4. concentrationAfter concentration in vacuo the reaction mixture
  5. additionadded
  6. customThe organic layer is separated
  7. washwashed well with water
  8. customdried
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-4cd594dcde664b1a848c4bc6ba80611b
출처 데이터셋
uspto-grants-1980_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04217352

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