Water → 2',5-Dichloro-2-methylaminobenzhydrol

HRID 617085노트

반응식

HRID 617085 반응식
[BH4-].[Na+].[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[C:10](=[O:20])[C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[NH:18][CH3:19].O>O1CCCC1>[Cl:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[CH:10]([OH:20])[C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:12]=1[NH:18][CH3:19]

참가 물질

5

반응물 3

HCID 962Water2회HCID 21833Benzophenone, 2',5-dichloro-2-methylamino-HCID 4311764Sodium borohydride

생성물 1

HCID 124217352',5-Dichloro-2-methylaminobenzhydrol수율 97.1%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a suspension of sodium borohydride (1.2 g) in tetrahydrofuran (10 ml), a solution of 2', 5-dichloro-2-methylaminobenzophenone (3.12 g) in tetrahydrofuran (20 ml) is added dropwise. The resultant mixture is mixed with water (5 ml) and stirred at room temperature overnight. The reaction mixture is mixed with a small amount of water and evaporated under reduced pressure to remove the solvent. The residue is made to pH 8-9 with dilute hydrochloric acid and shaken with chloroform. The organic layer is dried and evaporated to give 2',5-dichloro-2-methylaminobenzhydrol (3.05 g). This substance is recrystallized from ether/n-hexane to give crystals melting at 105.5° to 106.5° C. The yield is 97.1 %.

후처리

  1. customevaporated under reduced pressure
  2. customto remove the solvent
  3. stirringshaken with chloroform
  4. customThe organic layer is dried
  5. customevaporated

출처 및 근거

ORD 기록
ord-d8f9d5d01c834c4c8e15995299f7b992
출처 데이터셋
uspto-grants-1978_02
특허 번호
US04076705

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