Ammonia → (R*,R*)-N-[5-[1-Hydroxy-2-[[2-(4-methoxyphenyl)-1-methylethyl](phenylmethyl)amino]ethyl]-2-(phenylmethoxy)phenyl]formamide

HRID 572704노트

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HRID 572704 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][C:29]=1[O:30][CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)[CH:5]([OH:26])[CH2:6][N:7]([CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)[CH:8]([CH3:18])[CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=1.C1C[O:41][CH2:40]C1.C(OC=O)(=O)C.N>C1(C)C=CC=CC=1>[CH2:31]([O:30][C:29]1[CH:28]=[CH:27][C:4]([CH:5]([OH:26])[CH2:6][N:7]([CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:8]([CH3:18])[CH2:9][C:10]2[CH:11]=[CH:12][C:13]([O:16][CH3:17])=[CH:14][CH:15]=2)=[CH:3][C:2]=1[NH:1][CH:40]=[O:41])[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8028TetrahydrofuranHCID 75269Acetic-formic anhydrideHCID 54335918HCID 54335918, 화합물

생성물 1

HCID 11734094(R*,R*)-N-[5-[1-Hydroxy-2-[[2-(4-methoxyphenyl)-1-methylethyl](phenylmethyl)amino]ethyl]-2-(phenylmethoxy)phenyl]formamide

시약·촉매·용매 1

HCID 1140Toluene용매2회

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온도
15 °C

실험 절차

3-amino-4-benzyloxy-α-[N-benzyl-N-(1-methyl-2-p-methoxyphenylethyl)aminomethyl]benzyl alcohol (100 gms, 0.2 M), toluene 0.2 lit and 0.2 lit THF, were charged in a reactor. The reaction mass was cooled to 15° C. and 35 ml of 3:2 formic acid-acetic anhydride was introduced maintaining temperature below 20° C. The reaction mass was further stirred at 20-30° C. for 1 hour and concentrated under reduced pressure. The residue obtained was dissolved in toluene (0.65 lit) and basified with liquor ammonia. The organic layer was separated, washed with water and concentrated under reduced pressure below 35° C. to yield the title compound. (100 gms, 94.66%)

후처리

  1. additionwere charged in a reactor
  2. temperaturemaintaining temperature below 20° C
  3. concentrationconcentrated under reduced pressure
  4. customThe residue obtained
  5. customThe organic layer was separated
  6. washwashed with water
  7. concentrationconcentrated under reduced pressure below 35° C.

출처 및 근거

ORD 기록
ord-e56bb5d09cad452faad9466d50efa315
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09029421B2

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