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Dichloromethane → HCID 86595789, 화합물

HRID 1241449
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HRID 1241449 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C@@H:10]([CH2:17][C:18]3[N:19]=[C:20]([CH2:23][CH2:24][CH2:25][CH:26]=O)[S:21][CH:22]=3)[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:9][C:4]=2[O:3][CH2:2]1.[N:28]1([C:34]2[CH:39]=[CH:38][N:37]=[C:36]([NH2:40])[CH:35]=2)[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1.C1COCC1.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+].C(Cl)[Cl:61]>>[ClH:61].[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C@@H:10]([CH2:17][C:18]3[N:19]=[C:20]([CH2:23][CH2:24][CH2:25][CH2:26][NH:40][C:36]4[CH:35]=[C:34]([N:28]5[CH2:33][CH2:32][O:31][CH2:30][CH2:29]5)[CH:39]=[CH:38][N:37]=4)[S:21][CH:22]=3)[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:9][C:4]=2[O:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 6344DichloromethaneHCID 8028TetrahydrofuranHCID 5049666Sodium triacetoxyborohydride2회HCID 219345374-(Morpholin-4-yl)pyridin-2-amineHCID 86595788HCID 86595788, 화합물

생성물 1

HCID 86595789HCID 86595789, 화합물

실험 절차

Dissolve (3S)-Ethyl 3-(1,3-benzodioxol-5-yl)-4-[2-(4-oxobutyl)-1,3-thiazol-4-yl]butanoate (230 mg, 0.6 mmol) and 4-morpholin-4-ylpyridin-2-amine (88 mg, 0.5 mmol) prepared according to Scheme 6, Example 1, in CH2Cl2. Add 3 mL THF and add NaBH(OAc)3. Stir at room temperature for 18 hours. Add 1.0 eq NaBH(OAc)3 and stir 24 hrs. The reaction was concentrated in vacuo and purified via reverse phase HPLC using a gradient of 10–60% CH3CN/H2O/0.5% HCl over 30 minutes to obtain the crude desired product.

후처리

  1. customprepared
  2. stirringstir 24 hrs
  3. concentrationThe reaction was concentrated in vacuo
  4. custompurified via reverse phase HPLC
  5. customover 30 minutes

출처 및 근거

ORD 기록
ord-03a1df963e514719a66a7cb809f25ad0
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07115596B2

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