Water → HCID 13577659, 화합물

HRID 1589210노트

반응식

HRID 1589210 반응식
[NH2:1][C:2]1[C:7]([C:8](=[O:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][C:18](OCC)=[O:19].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:1][C:2]1[C:7]([CH:8]([OH:15])[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=[CH:6][C:5]([Cl:16])=[CH:4][C:3]=1[CH2:17][CH2:18][OH:19]

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 13577656HCID 13577656, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 13577659HCID 13577659, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 15.85 g (0.05 mole) of 2-amino-3-benzoyl-5-chlorobenzeneacetic acid, ethyl ester dissolved in 100 ml of dry tetrahydrofuran was added dropwise to a suspension of 4.0 g (0.105 mole) of lithium aluminum hydride in 50 ml of dry tetrahydrofuran. Gentle reflux was maintained during the addition. Reflux was continued for 2 hours after completion of the addition. The mixture was cooled and carefully treated with 4 ml of water, 4 ml of 15% sodium hydroxide and 12 ml of water. The resulting mixture was filtered, the filtrate stripped and the resulting residue recrystallized from toluene. The titled compound, 10.5 g (70%) having a m.p. of 130°-132° C. was obtained.

후처리

  1. temperatureGentle reflux
  2. temperaturewas maintained during the addition
  3. temperatureReflux
  4. additionafter completion of the addition
  5. temperatureThe mixture was cooled
  6. filtrationThe resulting mixture was filtered
  7. customthe resulting residue recrystallized from toluene
  8. customwas obtained

출처 및 근거

ORD 기록
ord-407d037d476946e0858e390a2667ff4e
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04568695

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